• Title/Summary/Keyword: Fourier transformation - infrared spectroscopy

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A Method for Absolute Determination of the Surface Areal Density of Functional Groups in Organic Thin Films

  • Min, Hyegeun;Son, Jin Gyeong;Kim, Jeong Won;Yu, Hyunung;Lee, Tae Geol;Moon, Dae Won
    • Bulletin of the Korean Chemical Society
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    • v.35 no.3
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    • pp.793-797
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    • 2014
  • To develop a methodology for absolute determination of the surface areal density of functional groups on organic and bio thin films, medium energy ion scattering (MEIS) spectroscopy was utilized to provide references for calibration of X-ray photoelectron spectroscopy (XPS) or Fourier transformation-infrared (FT-IR) intensities. By using the MEIS, XPS, and FT-IR techniques, we were able to analyze the organic thin film of a Ru dye compound ($C_{58}H_{86}O_8N_8S_2Ru$), which consists of one Ru atom and various stoichiometric functional groups. From the MEIS analysis, the absolute surface areal density of Ru atoms (or Ru dye molecules) was determined. The surface areal densities of stoichiometric functional groups in the Ru dye compound were used as references for the calibration of XPS and FT-IR intensities for each functional group. The complementary use of MEIS, XPS, and FT-IR to determine the absolute surface areal density of functional groups on organic and bio thin films will be useful for more reliable development of applications based on organic thin films in areas such as flexible displays, solar cells, organic sensors, biomaterials, and biochips.

Bioactivity of $CaO-P_2O_5-SiO_2$ Glasses ($CaO-P_2O_5-SiO_2$계 유리의 생체활성)

  • 조정식;김철영
    • Journal of the Korean Ceramic Society
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    • v.30 no.6
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    • pp.433-440
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    • 1993
  • The bioactivity of glasses in the CaO-SiO2 system and CaO-P2O5-SiO2 system with less than 10mol% of P2O5 was investigated by in vitro test in simulated body flood(SBF). The formation of Ca.P film and hydroxyapatite on the surface of glasses after in vitro test was analysed by X-ray photoelectron spectoscopy (XPS), fourier transform infrared reflection spectroscopy (FT-IRRS), energy dispersive X-ray spectroscopy (EDS), and scanning electron microscopy (SEM) observation. In the early stage of Ca.P film formation after in vitro test for CaO-SiO2 and CaO-P2O5-SiO2 glasses, the rate of Ca.P film formation on the surface of the glasses was dependent of structural parameter (Y) evaluated from the glass composition. First, in the case of the glasses having Y value below 2, Ca.P film and SiO2-rich layer were formed simultaneously, and there were no differences of the rate of Ca.P film formation in terms of the Y values. Second, in the case of the glasses having Y value above 2, the SiO2-rich layer was formed, and then Ca.P.Si mixed layer was formed in the silica gel structure of the SiO2-rich layer, and finally the Ca.P film on the surface of SiO2-rich layer. The rate of Ca.P film formation delayed as the Y values increased. The rate of hydroxyapatite formation of glasses (the rate of transformation from Ca.P film to hydroxyapatite) seems to be propotional to the rate of Ca.P film formation and Y value. The rate of hydroxyapatite formation of glasses belonging to the second group was delayed as structural parameter increased, and the hydroxyapatite crystal showed spherical growth in the early reaction stage, and then showed silkworm-like linear growth as the reaction time increased.

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Effect of B2O3 Additives on GaN Powder Synthesis from GaOOH (GaOOH로부터 GaN 분말의 합성에 미치는 B2O3의 첨가효과)

  • Song, Changho;Shin, Dongwhee;Byun, Changsob;Kim, Seontai
    • Korean Journal of Materials Research
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    • v.23 no.2
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    • pp.104-111
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    • 2013
  • In this study, GaN powders were synthesized from gallium oxide-hydroxide (GaOOH) through an ammonification process in an $NH_3$ flow with the variation of $B_2O_3$ additives within a temperature range of $300-1050^{\circ}C$. The additive effect of $B_2O_3$ on the hexagonal phase GaN powder synthesis route was examined by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Fourier transformation infrared transmission (FTIR) spectroscopy. With increasing the mol% of $B_2O_3$ additive in the GaOOH precursor powder, the transition temperature and the activation energy for GaN powder formation increased while the GaN synthesis limit-time ($t_c$) shortened. The XPS results showed that Boron compounds of $B_2O_3$ and BN coexisted in the synthesized GaN powders. From the FTIR spectra, we were able to confirm that the GaN powder consisted of an amorphous or cubic phase $B_2O_3$ due to bond formation between B and O and the amorphous phase BN due to B-N bonds. The GaN powder synthesized from GaOOH and $B_2O_3$ mixed powder by an ammonification route through ${\beta}-Ga_2O_3$ intermediate state. During the ammonification process, boron compounds of $B_2O_3$ and BN coated ${\beta}-Ga_2O_3$ and GaN particles limited further nitridation processes.

Bayberry Tannin as Stabilizer for the Synthesis of Highly Active and Reusable Heterogeneous Pd Catalysts and Their Application in the Catalytic Hydrogenation of Olefins

  • Chen, Chen;Lv, Guang;Huang, Xin;Liao, Xue Pin;Zhang, Wen Hua;Shi, Bi
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.403-408
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    • 2012
  • In this study, the homogenous Pd nanoparticles (Pd NPs) were first prepared with bayberry tannin (BT) as the stabilizers. Subsequently, the obtained bayberry tannin-stabilized Pd nanoparticles (BT-Pd) were immobilized onto ${\gamma}-Al_2O_3$ to prepare heterogeneous ${\gamma}-Al_2O_3$-BT-Pd catalysts. Fourier Transformation Infrared Spectrum (FTIR) and X-ray Photoelectron Spectroscopy (XPS) analyses confirmed that the Pd NPs were well stabilized by the phenolic hydroxyl groups of BT. Transmission Electron Microscopy (TEM) observation indicated that the diameter of the Pd NPs can be effectively controlled in the range of 4.2-16.0 nm by varying the amount of BT. It is found that the ${\gamma}-Al_2O_3$-BT-Pd catalysts exhibit highly activity for various olefin hydrogenations. For example, the initial TOF (turnover frequency) of the ${\gamma}-Al_2O_3$-BT-Pd in the allyl alcohol hydrogenation is as high as $12804 mol{\cdot}mol^{-1}{\cdot}h^{-1}$. Furthermore, the ${\gamma}-Al_2O_3$-BT-Pd can be reused 5 times without significant loss of activity, exhibiting a superior reusability as compared with conventionally prepared ${\gamma}-Al_2O_3$-Pd catalysts.

Use of FT-IR to Identify Enhanced Biomass Production and Biochemical Pool Shifts in the Marine Microalgae, Chlorella ovalis, Cultured in Media Composed of Different Ratios of Deep Seawater and Fermented Animal Wastewater

  • Kim, Mi-Kyung;Jeune, Kyung-Hee
    • Journal of Microbiology and Biotechnology
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    • v.19 no.10
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    • pp.1206-1212
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    • 2009
  • Growth rates, photosystem II photosynthesis, and the levels of chlorophyll $\alpha$ and secondary metabolites of Chlorella ovalis were estimated to determine if they were enhanced by the addition of swine urine (BM) or cow compost water (EP) that had been fermented by soil bacteria to deep seawater (DSW) in an attempt to develop media that enabled batch mass culture at lower costs. Growth of C. ovalis in f/2, f/2-EDTA+BM60%, DSW+BM30%, and DSW+EP60% was enhanced and maintained in the log phase of growth for 16 days. The cell densities of C. ovalis in DSW+EP60% ($4.1{\times}10^6$ Cells/ml) were higher than those of f/2 ($2.9{\times}10^6$ Cells/ml), f/2-E+BM60% ($3.7{\times}10^6$ Cells/ml), and DSW+BM30% ($2.7{\times}10^6$ Cells/ml). The growth rate was also more favorable for C. ovalis cultured in DSW+EP60% ($0.15\;day^{-1}$) than that of C. ovalis cultured in the control medium (f/2) ($0.12\;day^{-1}$). Furthermore, the chlorophyll a concentration of C. ovalis cultured in DSW+EP60% (4.56 mg/l) was more than 2-fold greater than that of C. ovalis cultured in f/2 (2.35 mg/l). Moreover, the maximal quantum yields of photo system II at 470 nm (Fv/Fm) were significantly higher in organisms cultured at f/2-E+BM60% (0.53) and DSW+EP60% (0.52) than in the other treatment groups. Finally, Fourier transformation infrared (FT-IR) spectroscopy revealed that C. ovalis grown in DSW+EP60% had more typical peaks and various biochemical pool shifts than those grown in other types of media. Taken together, the results of this study indicate that the use of DSW+EP60% to culture C. ovalis can reduce maintenance expenses and promote higher yields.

The Powder Preparation of Blue Cobalt Aluminate at 210 °C Using the Malonate Method

  • Lee, Gong-Yeol;Lee, Dong-Hoon;Kim, Hong-Gun;Kim, Yoo-Young
    • Bulletin of the Korean Chemical Society
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    • v.31 no.1
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    • pp.47-51
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    • 2010
  • A powder, containing 80 percent of blue cobalt aluminate $(CoAl_2O_4)$ crystallites, was synthesized at $210 ^{\circ}C$ using a (metal nitrate-malonic acid-ammonium hydroxide-ammonium nitrate) system. The optimal amount of concentrated ammonia water and initial decomposition temperature were determined for the blue $CoAl_2O_4$ crystallites preparation. Three $CoAl_2O_4$ precursor pastes, corresponding to the various amounts of concentrated ammonia water, were prepared by evaporating the initial solutions in an electric furnace fixed at $80 ^{\circ}C$ under a vacuum of 25 torr. The initial solution was used to dissolve the starting materials. The powder with the maximum content (80%) of blue $CoAl_2O_4$ crystallites was prepared when the prepared precursor was decomposed at $210 ^{\circ}C$. The blue $CoAl_2O_4$ crystallite content in the prepared sample decreased with increasing initial decomposition temperature. For 0.2 mole of the $Al^{3+}$ ion, the chemical compositions of the precursor corresponded to molar ratios of 0.4, 1.40, 2.56 and 2.00 for the $Co^{2+}$ ion, malonic acid, ammonia and ammonium nitrate per mole of the $Al^{3+}$ ion, respectively. The blue $CoAl_2O_4$ crystallite content in the sample decreased with the amount of ammonia deviated from the optimal value. The characteristics of the powders were examined using X-ray diffraction, optical microscopy, Fourier transformation infrared spectroscopy and the Brunauer-Emmett-Teller technique.

The polymerization efficiency of a bulk-fill composite based on matrix-modification technology

  • Elshazly, Tarek M.;Bourauel, Christoph;Aboushelib, Moustafa N.;Sherief, Dalia I.;El-Korashy, Dalia I.
    • Restorative Dentistry and Endodontics
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    • v.45 no.3
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    • pp.32.1-32.12
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    • 2020
  • Objectives: To evaluate the polymerization efficiency of a matrix-modified bulk-fill composite, and compare it to a conventional composite which has a similar filler system. The degree of conversion (DC%) and monomer elution were measured over different storage periods. Additionally, fillers' content was examined. Materials and Methods: Cylindrical specimens were prepared, in bulk and incrementally, from Filtek Bulk Fill (B) and Filtek Supreme XTE (S) composites using a Teflon mold, for each test (n = 6). Using attenuated total reflection method of Fourier transformation infrared spectroscopy, DC% was measured after 24 hours, 7 days, and 30 days. Using high-performance liquid chromatography, elution of hydroxyethyl methacrylate, triethylene glycol dimethacrylate, urethane dimethacrylate, and bisphenol-A glycidyl dimethacrylate was measured after 24 hours, 7 days and 30 days. Filler content was examined by scanning electron microscopy (SEM). Data were analyzed using 2-way mixed-model analysis of variance (α = 0.05). Results: There was no significant difference in DC% over different storage periods between B-bulk and S-incremental. Higher monomer elution was detected significantly from S than B. The elution quantity and rate varied significantly over storage periods and between different monomers. SEM images showed differences in fillers' sizes and agglomeration between both materials. Conclusions: Matrix-modified bulk-fill composites could be packed and cured in bulk with polymerization efficiency similar to conventional composites.

Characterization and Photocatalytic effect of ZnO nanoparticles synthesized by spray-pyrolysis method

  • Lee, Sang-Duck;Nam, Sang-Hun;Kim, Myoung-Hwa;Lee, Kang-Suk;Kim, Young-Dok;Boo, Jin-Hyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.101-101
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    • 2010
  • ZnO shows a direct band gap of 3.37eV, large exciton binding energy (~60 meV), high oxidation ability, high sensitivity to many gases, and low cost, and it has been used in various applications such as transparent electrodes, light emitting diodes (LEDs), gas sensors and photocatalysts. Among these applications ZnO as photocatalyst has considerably attracted attention over the past few years because of its high activities in removing organic contaminants generated from industrial activities. In this research, ZnO nanoparticles were synthesized by spray-pyrolysis method using the zinc acetate dihydrate as starting material at synthesis temperature of $900^{\circ}C$ with concentration varied from 0.01 to 1.0M. The physical and chemical properties of the synthesized ZnO nanoparticles were examined by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Fourier Transformation Infrared (FT-IR), and UV-vis spectroscopy. The Miller indices of XRD patterns indicate that the synthesized ZnO nanoparticles showed a hexagonal wurtzite structure. With increased precursor concentration, a primary, secondary particle sizes of ZnO nanoparticles increased by 0.8 to $1.5{\mu}m$ and 15 to 35nm, and their crystallinity was improved. Methyleneblue (MB) solution ($1{\mu}M$) as a test comtaminant was prepared for evaluating the photocatalytic activities of ZnO nanoparticles synthesized in different precursor concentration. The results show that the photocatalytic efficiency of ZnO nanoparticles was gradually enhanced by increased precursor concentration.

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Hydrogeneted Amorphous Carbon Nitride Films on Si(100) Deposited by DC Saddle Field Plasma Enhanced Chemical Vapor Deposition ($N_2/CH_4$가스비에 따른 Hydrogenated Amorphous Carbon Nitride 박막의 특성)

  • 장홍규;김근식;황보상우;이연승;황정남;유영조;김효근
    • Journal of the Korean Vacuum Society
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    • v.7 no.3
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    • pp.242-247
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    • 1998
  • Hydrogenated amorphous carbon nitride[a-C:H(N)] films were deposited on p-type Si(100) at room temperature with bias voltage of 200 V by DC saddle-field plasma-enhanced chemical vapor deposition. Effects of the ratio of $N_2$ to $CH_4$($N_2/CH_4$), in the range of 0 and 4 on such properties as optical properties, microstucture, relative fraction of nitrogen and carbon, etc. of the films have been investigated. The thickness of the a-C:H(N) film was abruptly decreased with the addition of nitrogen, but at $N_2/CH_4$>0.5, the thickness of the film gradually decreased with the increase of the $N_2/CH_4$. The ratio of N to C(N/C) of the films was saturated at 0.25 with the increase of $N_2CH_4$. N-H, C≡N bonds of the films increased but C-H bond decreased with the increase of $N_2CH_4$.Optical band gap energy of the film decreased from 2.53 eV at the ratio of $N_2CH_4$=4.

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Fabrication and Photocatalytic Properties of SiO2-TiO2 Composite Nanofibers (SiO2-TiO2계 복합 나노섬유의 제조 및 광활성 연구)

  • Hyun, Dong Ho;Lim, Tae-Ho;Lee, Sung Wook
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.554-558
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    • 2008
  • $(1-x)SiO_2-(x)TiO_2$ composite fibers with various compositions of $TiO_2$ were prepared by electrospinning their sol-gel precursors of titanium (IV) iso-propoxide (TiP), and tetraethyl orthosilicate (TEOS). The surface morphology and structure of sintered composite fibers were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), simultaneous thermogravimetric analysis-differential scanning calorimetry (TGA-DSC) and Fourier transform infrared spectroscopy (FT-IR). As the content of $TiO_2$ in $(1-x)SiO_2-(x)TiO_2$ system was increased the average diameter of composite fibers was proportionally increased. Also, the transformation of $TiO_2$ from anatase to rutile form was inhibited by the highly dispersed $TiO_2$ around $SiO_2$ particles up to $0.6SiO_2-0.4TiO_2$ composite fibers even after calcination at $1000^{\circ}C$. The photocatalytic activity of $SiO_2-TiO_2$ composite fibers was examined for the methylene blue (MB) decomposition which was confirmed using UV-vis/DRS spectra. The experiments demonstrated that the MB in aqueous solution was successfully photodegraded using $SiO_2-TiO_2$ composite nanofibers under UV-visible light irradiation.