• Title/Summary/Keyword: XRD and FT-IR

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Graphene Based Cu Oxide Nanocomposites for C-N Cross Coupling Reaction

  • Choi, Jong Hoon;Park, Joon B.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.138.2-138.2
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    • 2013
  • Copper oxide is a multi-functional material being used in various research areas including catalysis, electrochemical materials, oxidizing agents etc. Among these areas, we have synthesized and utilized graphene based copper oxide nanocomposites (CuOx/Graphene) for the catalytic applications (C-N cross coupling reaction). Briefly, Cu precursors were anchored on the graphite oxide(GO) sheets being exfoliated and oxidized from graphite powder. Two different crystalline structures of Cu2O and CuO on graphene and GO were prepared by annealing them in Ar and O2 environments, respectively. The morphological and electronic structures were systemically investigated using FT-IR, XRD, XPS, XAFS, and TEM. Here, we demonstrate that the catalytic performance was found to depend on oxidative states and morphological structures of CuOx graphene nanocomposites. The relationship between the structure of copper oxides and catalytic efficiency toward C-N cross coupling reaction will be discussed.

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Preparation of Carrageenan-based Antimicrobial Films Incorporated With Sulfur Nanoparticles

  • Saedi, Shahab;Shokri, Mastaneh;Rhim, Jong-Whan
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.26 no.3
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    • pp.125-131
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    • 2020
  • Carrageenan-based functional films were prepared by adding two different types of sulfur nanoparticles (SNP) synthesized from sodium thiosulfate (SNPSTS) and elemental sulfur (SNPES). The films were characterized using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction spectroscopy (XRD), and thermal gravimetric analysis (TGA). Also, film properties such as UV-visible light transmittance, water contact angle (WCA), water vapor permeability (WVP), mechanical properties, and antibacterial activity were evaluated. SNPs were uniformly dispersed in the carrageenan matrix to form flexible films. The addition of SNP significantly increased the film properties such as water vapor barrier and surface hydrophobicity but did not affect the mechanical properties. The carrageenan/SNP composite film showed some antibacterial activity against foodborne pathogenic bacteria, L. monocytogenes and E. coli.

Highly efficient adsorptive removal of uranyl ions from aqueous solutions using dicalcium phosphate nanoparticles as a superabsorbent

  • Saghatchi, Hadis;Ansari, Reza;Mousavi, H. Zavvar
    • Nuclear Engineering and Technology
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    • v.50 no.7
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    • pp.1112-1119
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    • 2018
  • Dicalcium phosphate nanoparticles (DCP-NPs) was synthesized chemically and used for adsorptive removal of uranyl ions from aqueous solutions in a batch system. A commercial grade of DCP (monetite) was also employed for comparison. The synthesized and commercial adsorbents (S-DCP and C-DCP) were characterized by FT-IR, SEM and XRD techniques. The investigation of adsorption isotherms indicated that the maximum adsorption capacities ($q_m$) for C-DCP and S-DCP were 714.3 and $666.7mg\;g^{-1}$ (at 293 K), respectively. The experimental kinetics were well-described by the pseudo-second-order kinetic and the equilibrium data were fitted with both Langmuir and Freundlich adsorption models. Thermodynamic studies indicated that the adsorption of uranyl ions on the monetite surface was a spontaneous exothermic process. The exhausted adsorbents could be regenerated by washing with $0.10mol\;L^{-1}$ NaOH.

High Selective Oxidation of Alcohols Based on Trivalent Ion (Cr3+ and Co3+) Complexes Anchored on MCM-41 as Heterogeneous Catalysts

  • Shojaei, Abdollah Fallah;Rafie, Mahboubeh Delavar;Loghmani, Mohammad Hassan
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2748-2752
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    • 2012
  • Cr(III) and Co(III) complexes with acetylacetonate were anchored onto a mesoporous MCM-41 through Schiff condensation. The materials were characterized by XRD, FT-IR, BET, CHN and ICP techniques. Elemental analysis of samples revealed that one C=N bond was formed through Schiff condensation on MCM-41 surface. The catalysts were tested for the alcohol oxidations using t-butyl hydroperoxide (TBHP) and $H_2O_2$ as oxidant. The catalytic experiments were carried out at both room temperature and reflux condition. Various solvents such as dichloromethane, acetonitrile and water were examined in the oxidation of alcohols. Among the different solvents, catalytic activity is found more in acetonitrile. Further, the catalysts were recycled three times in the oxidation of alcohols and no major change in the conversion and selectivity is observed, which shows that the immobilized metal-acetylacetonate complexes are stable under the present reaction conditions.

Synthesis of Poly Imide/α'ω'-di Poly Acrylamide (3-Mercaptopropyl) Trimethoxysilane Terminated Copolymer (양 말단에 MPTMS-아크릴아미드로 치환된 폴리이미드의 합성)

  • Min, Jun Ho;Park, Chan Young;Min, Seong Kee
    • Korean Journal of Materials Research
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    • v.26 no.9
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    • pp.478-485
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    • 2016
  • An amide group was introduced to restrain the cohesion of silica nano-particles and copolymerized with polyamic acid. Amide block copolymers were prepared using silica and (3-mercaptopropyl) trimethoxysilane (MPTMS) with a siloxane group, using 2, 6-Lutidine as a catalyst. Amide block polymers and copolymers were synthesized via ATRP after brominating pyromellitic dianhydride (PMDA) and polyamic acid of methylene diphenyl diamine (MDA) using ${\alpha}$-bromo isobutyryl bromide. Characteristic peaks of copolymer with amide and imide groups and patterns of amorphous polymers were studied using FT-IR and XRD analyses; an analysis of the surface characteristic groups was conducted via XPS. Changes in the thermal properties were examined through DSC and TGA; solubility for solvents was also studied.

Effect of Structural and Morphological Changes on the Conductivity of Stretched PANI-DBSA/HIPS Film

  • Lee, Jong-Hyeok;Kim, Eun-Ok
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2661-2665
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    • 2011
  • We studied the effect of structural and morphological changes on the conductivity of a stretched conducting polymer film. To improve the poor processability of polyaniline, we used dodecylbenzenesulfonic acid as both a surfactant and a dopant during emulsion polymerization, followed by blending with high-impact polystyrene. UV-Vis/NIR spectra were obtained to observe conformational changes, and SEM and AFM were used to investigate morphological changes. FT-IR dichroism was applied to determine the microscopic orientation, and XRD patterns were obtained for quantitative crystallinity analysis. The electrical conductivity (${\sigma}_{\parallel}/{\sigma}_{\perp}$) was measured as a function of draw ratio. We found a clear correlation between morphological changes and (${\sigma}_{\parallel}/{\sigma}_{\perp}$), especially at the stretching limit. The conductivity of the films can be modified according to the desired application by controlling their structure and morphology.

Enhanced Removal of Phenol from Aquatic Solution in a Schorl-catalyzed Fenton-like System by Acid-modified Schorl

  • Xu, Huan-Yan;Prasad, Murari;Wang, Peng
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.803-807
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    • 2010
  • Schorl modified by $H_2SO_4$ has been successfully developed to enhance schorl-catalyzed Fenton-like reaction for removal of phenol in an aqueous solution. The phenol removal percentage can be increased from 4% to 100% by the system of modified schorl and $H_2O_2$. Batch experiments indicate that the percent increases in removal of phenol by increasing the dosage of catalyst, temperature and initial concentration of $H_2O_2$. The results of XRD, FT-IR and SEM suggest that no new phases are formed after removal of phenol by modified schorl. ICP-AES results reveal that more dissolution of iron results in higher catalytic oxidant activity in the system of modified schorl and $H_2O_2$. Besides minor adsorption, mineral-catalyzed Fenton-like reaction governs the process.

High Catalytic Activity and Recyclability of Graphene Oxide Based Palladium Nanocomposites in Sonogashira Reaction

  • Kim, Bo Hyun;Park, Joon B.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.139.1-139.1
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    • 2013
  • Graphene and graphene oxide (GO) have been modified with palladium nanoparticles (Pd NPs) to develop high performance catalysts for the Sonogashira cross coupling reaction. To understand catalytic performance of Pd NPs on graphene (Pd/G) and Pd NPs on GO (Pd/GO), we monitored their morphological and electronic structural changes before/after Sonogashira reaction using FT-IR, XRD, XPS, and XAFS. Here, we demonstrate that both Pd/G and Pd/GO show high catalytic efficiency toward the Sonogashira reaction, but only Pd/GO revealed excellent recyclability. The remarkable catalytic efficiency of both catalysts is attributed to the high degree of the Pd NP dispersions on supports and thus smaller Pd NPs can provide highly reactive low coordinated Pd atoms. However, we attributed the excellent recyclability of Pd/GO to the presence of oxygen functionalities on GO, which can provide nucleation sites for the detached Pd atoms during the Sonogashira reaction and prevent agglomeration of the Pd NPs since the oxygen functional groups are very reactive to mobile Pd adatoms.

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Uranium Recovery from Nuclear Fuel Powder Conversion Plant Filtrate and its Thermal Decomposition Characteristics (핵연료분말 제조공정에서 발생된 여액으로부터 우라늄 회수 및 회수된 우라늄 화합물의 열분해 특성)

  • Jeong, Kyung-Chai;Jeong, Ji-Young;Kim, Byung-Ho;Kim, Tae-Joon;Choi, Jong-Hyeun
    • Journal of the Korean Ceramic Society
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    • v.39 no.2
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    • pp.204-209
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    • 2002
  • In this study, $UO_4{\cdot}2NH_4F$, the precipitates which has low solubility, was obtained by chemical precipitation method to recover and reuse the trace uranium from the liquid waste producing in AUC process and for this compound it was characterized by means of chemical analysis, TG-DTA, XRD and FT-IR analyses. This compound was analyzed as $UO_4{\cdot}2NH_4F$ and shape of this precipitate was hexagonal type, having the size of 2∼3 ${\mu}m$. Also, the intermediates were obtained as $UO_4F,\;UO_4,\;UO_3,\;and\;U_3O_8$ by the thermal decomposition over the temperature of 220, 310, 515 and 640$^{\circ}C$, respectively. It is concluded that under the condition of a constant heating rate of 5$^{\circ}C$/min in air atmosphere range of between room temperature and 800$^{\circ}C$, thermal decomposition reaction mechanism of $UO_4{\cdot}2NH_4F$ is as follow; $UO_4{\cdot}2NH_4F{\rightarrow}UO_4F{\rightarrow}UO_4{\rightarrow}UO_3{\rightarrow}U_3O_8$.

Effect of Sinter Additives on Sol-Gel Derived Alumina Fibres

  • Lakshmi, N.S.;Gnanam, F.D.
    • The Korean Journal of Ceramics
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    • v.6 no.2
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    • pp.159-163
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    • 2000
  • Alumina fibre has been synthesized successfully by sol-gel technique. Boehmite sol was prepared by hydrolyzing aluminium iso-propoxide and peptizing it with nitric acid. The stable sol thus obtained was used for fibre drawing when their viscosity reached the required value as a result of progress of the hydrolyzation and polycondensation reaction. The fibres dried at 11$0^{\circ}C$ for 12 hours were sintered at 1$600^{\circ}C$ for 5 hours. A reasonable sintered density with better microstructure and strength have been attained using 2 wt% of urea, magnesia and silica as sinter additives. Thermal analysis with sintering additives of 2 wt% and phase determination of the heat treated fibres using XRD and FT IR spectra confirms the phase transitions. The observation of surface and cross-section of the fibres were made using SEM. Fibres of uniform circular cross-section is obtained by fixing the shape in a setting solution.

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