• Title/Summary/Keyword: TEM Journal

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All-trans Retinoic Acid Release from Surfactant-free Nanoparticles of Poly(DL-lactide-co-glycolide)

  • Jeong, Young-Il;Kim, Don-Gon;Jang, Mi-Kyeong;Nah, Jae-Woon;Kim, Yong-Bae
    • Macromolecular Research
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    • v.16 no.8
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    • pp.717-724
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    • 2008
  • In this study, we prepared all-trans retinoic acid (ATRA)-encapsulated, surfactant-free, PLGA nanoparticles. The nanoparticles were formed by nanoprecipitation process, after which the solvent was removed by solvent evaporation or dialysis method. When a nanoparticle was prepared by the nanoprecipitation - solvent evaporation method, the nanoparticles were bigger than the nanoparticles of the nanoprecipitation - dialysis method, despite the higher although loading efficiency. Nanoparticles from the nanoprecipitation - dialysis method were smaller than 200 nm in diameter, while the loading efficiency was not significantly changed. Especially, nanoparticles prepared from DMAc, 1,4-dioxane, and DMF had a diameter of less than 100 nm. In the transmission electron microscopy (TEM) observations, all of the nanoparticles showed spherical shapes. The loading efficiency of ATRA was higher than 90% (w/w) at all formulations with exception of THF. The drug content was increased with increasing drug-feeding amount while the loading efficiency was decreased. In the drug release study, an initial burst was observed for $2{\sim}6$ days according to the variations of the formulation, after which the drug was continuously released over one month. Nanoparticles from the nanoprecipitation - dialysis method showed faster drug release than those from the nanoprecipitation - solvent evaporation method. The decreased drug release kinetics was observed at lower drug contents. In the tumor cell cytotoxicity test, ATRA-encapsulated, surfactant-free, PLGA nanoparticles exhibited similar cytotoxicity with that of ATRA itself.

Strength Change due to Plastic Deformation in Al 2024 Ultrafine Grained ECAP Metal (ECAP 성형가공한 Al 2024 초미세결정립 재료의 소성변형량에 따른 강도 변화)

  • Choi, Jeong-Woo;Ma, Young-Wha;Yoon, Kee-Bong
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.29 no.10 s.241
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    • pp.1407-1415
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    • 2005
  • Strength change of an over-aged A12024 material was studied after being subjected to stages of severe plastic deformation by ECAP (Equal Channel Angular Pressing). Various kinds of strength value were measured using the conventional tensile test, Rockwell and Vickers hardness and the SP (small punch) test Due to limitation of the specimen size, tension test in transverse direction could not be conducted. Hence, SP test was employed for assessing the strength in transverse direction. Based on TEM observation the measured strength characteristics were explained based on the relation between microstructure, dislocation and strength. As the number of ECAP pass increases, the strength of A12024 was also increased. However, considerable change of strength, which is generally predicted, was not observed in this study. For the strength in transverse direction even decrease of the strength was observed after 6 passes of ECAP. It was argued that this decrease was due to dynamic recovery of dislocation density during or after ECAP processes at $150^{\circ}C$. The strength assessment equation proposed by the authors in the previous paper was shown to be very accurate. This argument was supported by comparing the results of conventional tensile test with those of SP test. It was also pointed that the Rockwell har(3ness value seemed to be able to represent the strength in the transverse direction.

Effect of Unsaturation on the Stability of C18 Polyunsaturated Fatty Acids Vesicles Suspension in Aqueous Solution

  • Teo, Yin Yin;Misran, Misni;Low, Kah Hin;Zain, Sharifuddin Md.
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.59-64
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    • 2011
  • Degree of unsaturation in fatty acid molecules plays an important role in the formation of vesicles. Vesicle formation from C18 fatty acids with different amount of double bonds such as oleic acid, linoleic acid and linolenic acid with the incorporation of 1,2-dipalmitoyl-sn-glycerol-3-phosphoethanolamine-N-[methoxy(polyethylene glycol)-2000] (DPPE-PEG2000) have been examined by TEM. Critical vesicular concentrations (CVC) of the vesicle suspension are determined by turbidity and surface tension methods. The CVC of fatty acids increases when the amount of unsaturation in the alkyl chain increases. On the other hand, stability of vesicle suspension has been examined by using particle size and zeta potential at $30^{\circ}C$. There was a dramatic decrease in particle size measurement from mono-unsaturation to tri-unsaturation which could be due to the effect of fluidity in the membrane bilayer caused by different degree of unsaturation. The values of zeta potential for vesicles that were formed without the incorporation of DPPE-PEG2000 were in the range of -70 mV to -100 mV. It has been observed that the incorporation of DPPEPEG2000 to the vesicle reduces the magnitude of zeta potential. However, this phenomenon does not obviously seen in fatty acid vesicles formed by linoleate-linoleic acid and linolenate-linolenic acid. We therefore conclude that the addition of DPPE-PEG2000 does not effectively improve the stability of the linoleate-linoleic acid and linolenatelinolenic acid vesicle at pH 9.0 after the evaluation of their particle size and zeta potential over a period of 30 days. Although the vesicles formed were not stable for more than 10 days, they have displayed the potential in encapsulating the active ingredients such as vitamin E and calcein. The results show that the loading efficiencies of vitamin E are of encouraging value.

Ag2Se-Graphene/TiO2 Nanocomposites, Sonochemical Synthesis and Enhanced Photocatalytic Properties Under Visible Light

  • Meng, Ze-Da;Zhu, Lei;Ghosh, Trisha;Park, Chong-Yeon;Ullah, Kefayat;Nikam, Vikram;Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • v.33 no.11
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    • pp.3761-3766
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    • 2012
  • $Ag_2Se$-Graphene/$TiO_2$ composite was synthesized by a facile sonochemical method. The as-prepared products were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM) and UV-vis diffuse reflectance spectrophotometer. During the reaction, both of the reduction of graphene oxide and loading of $Ag_2Se$ and $TiO_2$ particles were achieved. The as-prepared $Ag_2Se$-Graphene/$TiO_2$ composites possessed great adsorptivity of dyes, extended light absorption range, and efficient charge separation properties simultaneously. Hence, in the photodegradation of rhodamine B (Rh.B), a significant enhancement in the reaction rate was observed with $Ag_2Se$-Graphene/$TiO_2$ composites, compared to the pure $TiO_2$. The high activity can be attributed to the synergetic effects of high charge mobility, and red shift in absorption edge of $Ag_2Se$-Graphene/$TiO_2$ composites.

One-pot Syntheses of Metallic Hollow Nanoparticles of Tin and Lead

  • Lee, Gae-Hang;Choi, Sang-Il;Lee, Young-Hwan;Park, Joo-T.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1135-1138
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    • 2009
  • Hollow Sn and Pb nanoparticles have been prepared by a rapid injection of an aqueous solution of $SnCl_2$- poly(vinylpyrrolidone) (PVP, surfactant) and $Pb(OAc)_2${\cdot}$3H_2O-PVP$ into an aqueous solution of sodium borohydride (reducing agent) in simple, one-pot reaction at room temperature under an argon atmosphere, respectively. The two hollow nanoparticles have been fully characterized by TEM, HRTEM, SAED, XRD, and EDX analyses. Upon exposure to air, the black Pb hollow nanoparticles are gradually transformed into a mixture of Pb, litharge (tetragonal PbO), massicot (orthorhombic PbO), and $Pb_5O_8$. The order and speed of mixing of the reactants between the metal precursor-PVP and the reductant solutions and stoichiometry of all the reactants are crucial factors for the formation of the two hollow nanocrystals. The Sn and Pb hollow nanoparticles were produced only when 1:(1.5-2) and 1:3 ratios of the Sn and Pb precursors to $NaBH_4$ were employed with a rapid injection, respectively.

Kinetic Study of the Visible Light-Induced Sonophotocatalytic Degradation of MB Solution in the Presence of Fe/TiO2-MWCNT Catalyst

  • Zhang, Kan;Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.6
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    • pp.1589-1595
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    • 2010
  • In order to effective degradation of organic dye both under visible light or ultrasonic irradiation, the MWCNTs (multiwalled carbon nanotube) deposited with Fe and $TiO_2$ were prepared by a modified sol-gel method. The Fe/$TiO_2$-MWCNT catalyst was characterized by surface area of BET, scanning electron microscope (SEM), Transmission Electron Microscope (TEM), X-ray diffraction (XRD), and energy dispersive X-ray (EDX) and ultraviolet-visible (UV-vis) spectroscopy. The low intensity visible light and low power ultrasound was as an irradiation source and the methylene blue (MB) was choose as the model organic dye. Then degradation experiments were carried out in present of undoped $TiO_2$, Fe/$TiO_2$ and Fe/$TiO_2$-MWCNT catalysts. Through the degradation of MB solution, the results showed the feasible and potential use of Fe/$TiO_2$-MWCNT catalyst under visible light and ultrasonic irradiation due to the enhanced formation of reactive radicals as well as the possible visible light and the increase of ultrasound-induced active surface area of the catalyst. After addition of $H_2O_2$, the MB degradation rates have been accelerated, especially with Fe/$TiO_2$-MWCNT catalyst, in case of that the photo-Fenton reaction occurred. The sonophotocatalysis was always faster than the respective individual processes due to the more formation of reactive radicals as well as the increase of the active surface area of Fe/$TiO_2$-MWCNT catalyst.

Moisture Absorption Characteristics of Pt/Nafion Membrane for PEMFC Prepared by a Drying Process (건식법에 의해 제조한 PEMFC용 Pt/나피온 막의 흡습 특성)

  • Lee, Jae-Young;Lee, Hong-Ki
    • Journal of Hydrogen and New Energy
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    • v.23 no.4
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    • pp.310-315
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    • 2012
  • A simple drying process was developed for the preparation of a Pt/Nafion self-humidifying membrane to be used for a proton-exchange membrane fuel cell (PEMFC). Platinum (II) bis (acetylacetonate), $Pt(acac)_2$ was sublimed, penetrated into the surface of a Nafion film and then reduced to Pt nanoparticles simultaneously without any support of a reducing agent in a glass reactor at $180^{\circ}C$ for 15 min. The process was carried out in $N_2$ atmosphere to prevent the oxidation of Pt nanoparticles at high temperature. The morphology and distribution of the Pt nanoparticles were observed by transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS), and we found that the average Pt particle size was ca. 3.7 nm, the penetration depth was ca. $17{\mu}m$. Almost all Pt nanoparticles were formed just beneath the surface and the number density decreased rapidly as the penetration depth increased. To estimate water absorption characteristics of the Nafion membranes, water uptake at an isothermal condition was measured by dynamic vapor sorption (DVS), and it was found that water uptake of the Pt/Nafion membrane was higher than that of the neat Nafion membrane.

Effect of Change of Hydrogen Rich Reductant on HC-SCR over Co-Pt/ZSM5 Catalyst (수소 풍부 환원제 변화가 Co-Pt/ZSM5 촉매를 사용하는 탈질 HC-SCR 반응에 미치는 영향)

  • Kim, Seong-Soo;Kim, Dae-Young;Oh, Se-Young;Yoo, Seong-Jeon;Sur, Young-Sek;Kim, Jin-Gul
    • Journal of Hydrogen and New Energy
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    • v.23 no.3
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    • pp.199-206
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    • 2012
  • HC-SCR was conducted over Co-Pt/ZSM5 catalyst coated over 200 cpsi cordierite in the condition of atomspheric pressure and $200^{\circ}C-500^{\circ}C$. Weight ratio of Co/Pt determined from EDX analysis was 8/2, which was almost equal to the weight ratio at preparation step. XPS showed that nitrates within cobalt precursor and chlorine withn Pt precursor were removed. TEM result demonstrated that crystallite size of cobalt and Pt was under 5nm. Among these tested hydrocarbon reductants, isobutane ($i-C_4H_{10}$) showed the highest de-$NO_x$ yield of 80% under the condition of the mole ratio of reductant/NOx=1.0 at $180^{\circ}C$. De-$NO_x$ yield from HC-SCR was increased as the carbon number of hydrocarbon reductant was increased. The decrease of bonding energy between C and H of HC reductant played a role to increase of de-$NO_x$ yield, which indicated that the dissociation step of C-H bond of hydrocarbon molecule might be the rate determining step of HC-SCR. The increase of oxygen concentration in the feed resulted in the decrease of de-$NO_x$ yield but the increase of CO and $N_2O$ yield.

Hydrogenation Properties of $Mg_2$Ni-(5, 10mass)$NbH_x$ Composites by Reactive Mechanical Alloying (기계적 합금화법에 의한 $Mg_2$Ni-(5, 10mass%)$NbH_x$ 복합재료의 수소화 특성)

  • Cho, Kyoung-Won;Park, Ji-Hee;Kim, Kyeong-Il;Kim, Soo-Hyun;Jung, Mi-Ewon;Kim, Sang-Hern;Choi, Jae-Ha;Hong, Tae-Whan
    • Journal of Hydrogen and New Energy
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    • v.20 no.6
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    • pp.512-518
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    • 2009
  • Mg 및 Mg합금은 수소 저장량이 7.6wt.%로 비교적 높고 자원도 풍부하여 값이 싼 장점을 가지고 있으나 산화반응성이 높고 활성화 에너지가 크기 때문에 반응온도가 높고 반응시간이 긴 단점을 가지고 있다. 이러한 단점을 극복하기 위해 일반적으로 Mg 및 Mg합금의 표면 개질화, 금속간 화합물 형성, 전이금속 첨가에 대한 연구가 활발히 진행되고 있다. 본 연구에서는 전이금속인 Nb를 촉매제로 사용하여 수소화 특성을 개선하고자 기계적 합금화법(MA;Mechanical Alloying)을 실시하여 복합재료를 합성한 후 수소화 반응을 평가하였다. XRD, SEM, TEM, PSA, TG/DSC 분석을 수행하였으며 Sievert's 형 PCT를 이용하여 온도 및 압력 변화에 따른 특성평가를 하였다. 전이금속인 Nb의 첨가로 수소화 반응개시온도가 낮아지고 수소 저장량이 향상되는 거동을 보였다. 특히, 5mass%Nb가 10mass%Nb 보다 수소 저장량 및 반응속도가 좋은 결과를 보였다.

Hydrogneation and Electrochemical Characteristics of Gas-atomized Zr-based $AB_2$ Hydride for Ni-MH Secondary Battery (기체분무형 공정으로 제조된 Zr계 금속수소화물의 수소화반응 및 Ni-MH 2차전지 전극 특성에 관한 연구)

  • Kim, Jin-Ho;Hwang, Kwang-Taek;Kim, Byung-Kwan;Han, Jeong-Seb
    • Journal of Hydrogen and New Energy
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    • v.20 no.6
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    • pp.505-511
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    • 2009
  • The hydriding and electrochemical characteristics of Zr-based $AB_2$ alloy produced by gas atomization have been extensively examined. For the particle morphology of the as-cast and gas-atomized powders, it can be seen that the mechanically crushed powders are irregular, while the atomized powder particles are spherical. The increase of jet pressure of gas atomization process results in the decrease of hydrogen storage capacity and the slope of plateau pressure significantly increases. TEM and EDS studies showed the increase of jet pressure in the atomization process accelerated the phase separation within grain of the gas-atomized alloy, which brought about a poor hydrogenation property. However, the gas-atomized $AB_2$ alloy powders produced by jet pressure of 50 bar kept up the reversible $H_2$ storage capacity and discharge capacity similar to the mechanically crushed particles. In addition, the electrode of gas-atomized Zr-based $AB_2$ alloy of 50 bar showed improved cyclic stability over that of the cast and crushed particulate, which is attributed to the restriction of crack propagation by grain boundary and dislocation with ch/discharging cycling.