• Title/Summary/Keyword: TEM Journal

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Preparation of Nanosized Palladium Oxide Powder with Average Particle Size Below 30 nm by Spray Pyrolysis Process (평균입도 30 nm 이하의 산화 팔라듐(PdO) 분체의 분무열분해공정에 의한 제조기술 개발)

  • Kim, Donghee;Yu, Jaekeun
    • Resources Recycling
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    • v.27 no.2
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    • pp.32-37
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    • 2018
  • This study was conducted as a preliminary study for the recycling of palladium and palladium oxide. In this study, thermodynamic equations for the formation of palladium oxide (PdO) are established. Palladium chloride is dissolved into hydrochloric acid to generate a palladium chloride solution. Nanosized palladium oxide powder with an average particle size below 30 nm were generated from this raw material solution by means of a spray pyrolysis process. The palladium oxide particles were composed of a single solid crystal. The results of XRD analysis showed that only a PdO phase of the generated powder was formed. And, the specific surface area of the generated palladium powder was approximately $32m^2/g$.

Gas Phase Oxidation of Toluene and Ethyl Acetate over Proton and Cobalt Exchanged ZSM-5 Nano Catalysts- Experimental Study and ANN Modeling

  • Hosseini, Seyed Ali;Niaei, Aligholi;Salari, Dariush;Jodaei, Azadeh
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.808-814
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    • 2010
  • Activities of nanostructure HZSM-5 and Co-ZSM-5 catalysts (with different Co-loading) for catalytic conversion of ethyl acetate and toluene were studied. The catalysts were prepared by wet impregnation method and were characterized by XRD, BET, SEM, TEM and ICP-AES techniques. Catalytic studies were carried out inside a U-shaped fixed bed reactor under atmospheric pressure and different temperatures. Toluene showed lower reactivity than ethyl acetate for conversion on Co-ZSM-5 catalysts. The effect of Co loading on conversion was prominent at temperatures below $400^{\circ}C$ and $450^{\circ}C$ for ethyl acetate and toluene respectively. In a binary mixture of organic compounds, toluene and ethyl acetate showed an inhibition and promotional behaviors respectively, in which the conversion of toluene was decreased at temperatures above $350^{\circ}C$. Inhibition effect of water vapor was negligible at temperatures above $400^{\circ}C$. An artificial neural networks model was developed to predict the conversion efficiency of ethyl acetate on Co-ZSM-5 catalysts based on experimental data. Predicted results showed a good agreement with experimental results. ANN modeling predicted the order of studied variable effects on ethyl acetate conversion, which was as follows: reaction temperature (50%) > ethyl acetate inlet concentration (25.085%) > content of Co loading (24.915%).

Synthesis of Cd1-xZnxS/K4Nb6O17 Composite and its Photocatalytic Activity for Hydrogen Production

  • Liang, Yinghua;Shao, Meiyi;Liu, Li;Hu, Jinshan;Cui, Wenquan
    • Bulletin of the Korean Chemical Society
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    • v.35 no.4
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    • pp.1182-1190
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    • 2014
  • $Cd_{1-x}Zn_xS$-sensitized $K_4Nb_6O_{17}$ composite photocatalysts (designated $Cd_{1-x}Zn_xS/K_4Nb_6O_{17}$) were prepared via a simple deposition-precipitation method. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectrometry (EDS), $N_2$ sorption, ultraviolet-visible light diffuse reflectance spectroscopy (UV-Vis DRS), photoluminescence measurements (PL), and X-ray photoelectron spectroscopy (XPS). The $Cd_{0.8}Zn_{0.2}S$ particles were scattered on the surface of $K_4Nb_6O_{17}$, and had a relatively uniform size distribution around 50 nm. The absorption edge of $K_4Nb_6O_{17}$ was shifted to the visible light region and the recombination of photo-generated electrons and holes suppressed after $Cd_{0.8}Zn_{0.2}S$ loading. The $Cd_{0.8}Zn_{0.2}S$(25 wt %)/$K_4Nb_6O_{17}$ composite possessed the highest photocatalytic activity for hydrogen production under visible light irradiation, evolving 8.278 mmol/g in 3 h. Recyclability tests were performed, and the composite photocatalysts were found to be fairly stable. The mechanism of charge separation between the photogenerated electrons and holes at the $Cd_{0.8}Zn_{0.2}S/K_4Nb_6O_{17}$ composite was discussed.

Doxorubicin Release from Core-Shell Type Nanoparticles of Poly(DL-lactide-co-glycolide)-Grafted Dextran

  • Jeong, Young-Il;Choi, Ki-Choon;Song, Chae-Eun
    • Archives of Pharmacal Research
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    • v.29 no.8
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    • pp.712-719
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    • 2006
  • In this study, we prepared core-shell type nanoparticles of a poly(DL-lactide-co-glycolide) (PLGA) grafted-dextran (DexLG) copolymer with varying graft ratio of PLGA. The synthesis of the DexLG copolymer was confirmed by $^1H$ nuclear magnetic resonance (NMR) spectroscopy. The DexLG copolymer was able to form nanoparticles in water by self-aggregating process, and their particle size was around $50\;nm{\sim}300\;nm$ according to the graft ratio of PLGA. Morphological observations using a transmission electron microscope (TEM) showed that the nanoparticles of the DexLG copolymer have uniformly spherical shapes. From fluorescence probe study using pyrene as a hydrophobic probe, critical association concentration (CAC) values determined from the fluorescence excitation spectra were increased as increase of DS of PLGA. $^1H-NMR$ spectroscopy using $D_2O$ and DMSO approved that DexLG nanoparticles have core-shell structure, i.e. hydrophobic block PLGA consisted inner-core as a drug-incorporating domain and dextran consisted as a hydrated outershell. Drug release rate from DexLG nano-particles became faster in the presence of dextranase in spite of the release rate not being significantly changed at high graft ratio of PLGA. Core-shell type nanoparticles of DexLG copolymer can be used as a colonic drug carrier. In conclusion, size, morphology, and molecular structure of DexLG nanoparticles are available to consider as an oral drug targeting nanoparticles.

Synthesis of N-Stearyl lactobionamide(N-SLBA) and Preparation of Neo-galactosylated Liposome (N-스테아릴락토비온아미드의 합성과 이를 이용한 리포좀의 제조)

  • Kim, Chong-Kook;Min, Mi-Hong;Min, Kyoung-Hee;Lah, Woon-Ryong;Lee, Bong-Jin;Kim, Yang-Bae
    • YAKHAK HOEJI
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    • v.36 no.2
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    • pp.159-166
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    • 1992
  • A neoglycolipid, N-stearyl lactobionamide(N-SLBA) was synthesized and the incorporation of the neoglycolipid into liposomes was achieved in order to prepare neo-galactosylated liposome as potential drug carrier for active targeting to galactose receptor existing cell and tissue. N-SLBA was synthesized by the covalent linkage between carboxyl group of lactobionic acid and amino group of stearylamine(SA). The yield of N-SLBA was about 52.3%. It was identified with $1650\;cm^{-1}$ in IR chart, 7.5 ppm in NMR spectra, $61^{\circ}C$ endothermic peak in DSC heating curve. Surface-modified large unilamellar vesicle with galactose(N-SLBA-LUV) could be prepared with N-SLBA by reverse evaporation method. N-SLBA-LUV was identified by TEM and measuring of membrane function. The maximum amount of N-SLBA incorporated into liposome is up to about 15 mol%. Compared with control liposome (SA-LUV), N-SLBA-LUV showed lower encapsulation efficiency of MTX. It might due to the loss of positive surface charge of stearylamine. N-SLBA-LUV was similar to SA-LUV in aspect of osmotic behavior. N-SLBA-LUV prepared with N-SLBA would be expected to be a good carrier for active targeting to galactose receptor existing cell and tissue.

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A Novel Acid-Base Catalyzed Sol-Gel Synthesis of Highly Active Mesoporous TiO2 Photocatalysts

  • Khan, Romana;Kim, Sun-Woo;Kim, Tae-Jeong;Lee, Hyo-Sun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.1951-1957
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    • 2007
  • A new synthetic strategy based on the acid-base catalyzed sol-gel method was developed for the preparation of a series of mesoporous TiO2 nanoparticles. A key feature of the method involves a gradual change in pH (0.8- 9) during the sol-gel transition, which guarantees easy introduction of mesoporosity without relying on the well-established sonochemical or template approach. In addition, this method leads to the exclusive formation of the anatase phase stable enough to the calcination temperature up to 600 oC. The physicochemical properties of the particles in the series were characterized by various spectroscopic and analytical techniques such as wide-angle XRD, SAXRD, BET surface area, FE-SEM, TEM, FT-IR, TGA, and XPS. The photocatalytic efficiency of these materials was investigated for the oxidation of toluene under UV-irradiation. All but T-ad in the series exhibited high photocatalytic activity pushing the reaction into completion within 3 h. The reaction followed the first order kinetics, and the rate reaches as high as 3.9 × 10?2/min which exceeds the one with the commercially available Degussa P-25 by a factor of 3.2. When comparison is made among the catalysts, the reactivity increases with increase in the calcination temperature which in turn increases the crystallinity of the anatase phase, thus revealing the following rate orders: T-3 < T-4 < T-5 < T-6.

Polystyrene-b-poly(oligo(ethylene oxide) Monomethyl Ether Methacrylate)-b-polystyrene Triblock Copolymers as Potential Carriers for Hydrophobic Drugs

  • You, Qianqian;Chang, Haibo;Guo, Qipeng;Zhang, Yudong;Zhang, Puyu
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.558-564
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    • 2013
  • A simple and effective method is introduced to synthesize a series of polystyrene-b-poly(oligo(ethylene oxide) monomethyl ether methacrylate)-b-polystyrene (PSt-b-POEOMA-b-PSt) triblock copolymers. The structures of PSt-b-POEOMA-b-PSt copolymers were characterized by Fourier-transform infrared spectroscopy (FTIR) and nuclear magnetic resonance ($^1H$ NMR) spectroscopy. The molecular weight and molecular weight distribution of the copolymer were measured by gel permeation chromatography (GPC). Furthermore, the self-assembling and drug-loaded behaviours of three different ratios of PSt-b-POEOMA-b-PSt were studied. These copolymers could readily self-assemble into micelles in aqueous solution. The vitamin E-loaded copolymer micelles were produced by the dialysis method. The micelle size and core-shell structure of the block copolymer micelles and the drug-loaded micelles were confirmed by dynamic light scattering (DLS) and transmission electron microscopy (TEM). The thermal properties of the copolymer micelles before and after drug-loaded were investigated by different scanning calorimetry (DSC). The results show that the micelle size is slightly increased with increasing the content of hydrophobic segments and the micelles are still core-shell spherical structures after drug-loaded. Moreover, the glass transition temperature (Tg) of polystyrene is reduced after the drug loaded. The drug loading content (DLC) of the copolymer micelles is 70%-80% by ultraviolet (UV) photolithography analysis. These properties indicate the micelles self-assembled from PSt-b-POEOMA-b-PSt copolymers would have potential as carriers for the encapsulation of hydrophobic drugs.

Synthesis and Characterization of Magnetic Nanoparticles and Its Application in Lipase Immobilization

  • Xu, Jiakun;Ju, Caixia;Sheng, Jun;Wang, Fang;Zhang, Quan;Sun, Guolong;Sun, Mi
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2408-2412
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    • 2013
  • We demonstrate herein the synthesis and modification of magnetic nanoparticles and its use in the immobilization of the lipase. Magnetic $Fe_3O_4$ nanoparticles (MNPs) were prepared by simple co-precipitation method in aqueous medium and then subsequently modified with tetraethyl orthosilicate (TEOS) and 3-aminopropyl triethylenesilane (APTES). Silanization magnetic nanoparticles (SMNP) and amino magnetic nanomicrosphere (AMNP) were synthesized successfully. The morphology, structure, magnetic property and chemical composition of the synthetic MNP and its derivatives were characterized using transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) analysis, X-ray diffraction, superconducting quantum interference device (SQUID) and thermogravimetric analyses (TGA). All of these three nanoparticles exhibited good crystallization performance, apparent superparamagnetism, and the saturation magnetization of MNP, SMNP, AMNP were 47.9 emu/g, 33.0 emu/g and 19.5 emu/g, respectively. The amino content was 5.66%. The AMNP was used to immobilize lipase, and the maximum adsorption capacity of the protein was 26.3 mg/g. The maximum maintained activity (88 percent) was achieved while the amount of immobilized lipase was 23.7 mg $g^{-1}$. Immobilization of enzyme on the magnetic nanoparticles can facilitate the isolation of reaction products from reaction mixture and thus lowers the cost of enzyme application.

Adsorptive removal of Ni(II) ions from aqueous solution by PVDF/Gemini-ATP hybrid membrane

  • Zhang, Guifang;Qin, Yingxi;Lv, Chao;Liu, Xingtian;Zhao, Yiping;Chen, Li
    • Membrane and Water Treatment
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    • v.7 no.3
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    • pp.209-221
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    • 2016
  • As a highly hydrophilic fibrillar mineral in nature, attapulgite (ATP) is a promising new additive for preparation of ultrafiltration (UF) hybrid membrane. In this work, ATP particles, which were grafted with a new Gemini surfactant of Ethyl Stearate-di(octadecyl dimethyl ammonium chloride) to detach the crystal bundles to single crystal and enhance the uniform dispersion in an organic polymer matrix, were incorporated into poly(vinylidene fluoride) (PVDF) matrix, and PVDF/Gemini-ATP hybrid membranes for adsorptive removal of Ni(II) ions from aqueous solution were prepared via a phase inversion method. Chemical composition, crystalization and morphology of the modified ATP were characterized by Fourier transform infrared spectroscopy (FTIR), Transmission electron microscope (TEM) and X-ray diffraction (XRD), respectively. The morphology of the hybrid membrane was characterized by Scanning electron microscopy (SEM), the performance of permeability, hydrophilicity and adsorption of Ni(II) ions were studied, and the adsorption kinetics of the PVDF/ATP hybrid membranes were particular concerned. The results showed that the hybrid membrane displayed a good thermal stability and hydrophilicity. Comparing with PVDF membrane, the hybrid membrane possessed good adsorption capacity for Ni(II) ions, and the adsorption kinetics fit well with Lagergren second-order equation.

Preparation of Aminosiloxane-grafted Poly(imidesiloxane) Copolymer and its Morphology and Adhesive Properties in Film (아미노실록산이 그래프팅된 폴리(이미드실록산) 공중합체 제조와 필름 모폴로지 및 점착 특성 연구)

  • Lee, Ji Mok;Kwon, Eunjin;Lee, Sunyoung;Jung, Hyun Min
    • Polymer(Korea)
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    • v.37 no.4
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    • pp.547-552
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    • 2013
  • Polyimide (PI) containing carboxyl functional group was prepared and reacted with diaminosiloxane during high temperature film casting. The morphology of resulting film was observed by using transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDX), which revealed that globular 100 nm-sized PI domains and continuous polysiloxane phase were formed. X-ray photoelectron spectroscopy (XPS) study indicated that air-film interface mainly consisted of polysiloxane blocks. Poly(imidesiloxane) thin layer was thermostable until $400^{\circ}C$ and its pressure- sensitive adhesive property was retained up to $300^{\circ}C$. The comparative experiments revealed that grafting between carboxyl groups of polyimide and aminosiloxane was crucial for formation of microdomain structure and pressure-sensitive adhesive property.