• Title/Summary/Keyword: Hydrothermal synthesis

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Syntheses and Structures of Two Reduced Open-framework Titanophosphates

  • Zhao, Yongnan;Yu, Jianguo;Kwon, Young-Uk
    • Bulletin of the Korean Chemical Society
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    • v.29 no.4
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    • pp.805-810
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    • 2008
  • Using metallic Ti powder as raw materials and 1,2-diaminocyclohexane (DACH) as the trial template, two novel reduced titanophosphate open-structures were hydrothermally isolated by varying the $H_3PO_4/H_2O$ ratio to adjust the pH value. TiPO-1 crystallizes in orthorhombic Pbca space group with cell parameters a = 21.956(3) $\AA$, b = 8.6268(11) $\AA$, c = 7.2883(9) $\AA$, V = 1380.5(3) $\AA^3$, Z = 4. TiPO-2 crystallizes in triclinic space group P$\bar{1}$ with parameters a = 5.1620(10) $\AA$, b = 8.815(2) $\AA$, c = 10.655(3) $\AA$, $\alpha$ = $99.45^{\circ}$, $\beta$ = $102.94^{\circ}$, $\gamma$ = $91.06^{\circ}$, V = 465.34 $\AA^3$. TiPO-1 is constructed by infinite -Ti-O-Ti-O- linkage that is capped by $PO_4$ groups to form a chain structure with protonated DACH molecules occupying the interchain spaces. TiPO-2 represents a rare 3-D reduced titanophosphate with 12-MR channels. The structure of TiPO-2 is a neutral framework with water molecules located in the channels.

Catalytic Gasification of Mandarin Waste Residue using Ni/CeO2-ZrO2

  • Kim, Seong-Soo;Kim, Jeong Wook;Park, Sung Hoon;Jung, Sang-Chul;Jeon, Jong-Ki;Ryu, Changkook;Park, Young-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3387-3390
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    • 2013
  • Catalytic gasification of mandarin waste residue was carried out using direct and indirect catalyst-contact methods for the first time. In the indirect method, non-catalytic reaction in a reactor was followed by catalytic upgrading of vapor product in another reactor. Two different catalysts, $Ni/{\gamma}-Al_2O_3$ and $Ni/CeO_2-ZrO_2$, were employed. $CeO_2-ZrO_2$ support was prepared using hydrothermal synthesis in supercritical water. The catalysts were characterized by $H_2$-temperature programmed reduction and Brunauer-Emmett-Teller analyses. Under the condition of equivalent ratio (ER) = 0, the indirect catalyst-contact method led to a higher gas yield than the direct method. Under ER = 0.2, the yield of biogas obtained over $Ni/CeO_2-ZrO_2$ was higher than that obtained over $Ni/{\gamma}-Al_2O_3$. Also, the coke formation of $Ni/CeO_2-ZrO_2$ was lower than that of $Ni/{\gamma}-Al_2O_3$. Such results were attributed to the higher reducibility and better lattice oxygen mobility of $Ni/CeO_2-ZrO_2$, which were advantageous for partial oxidation reaction.

Synthesis of Microporous Zeolitic Membranes and Application in Alcohol/water Separation (다공성 제올라이트 멤브레인의 합성 및 알코올 /물 분리에의 응용)

  • 김건중;남세종
    • Membrane Journal
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    • v.9 no.2
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    • pp.97-106
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    • 1999
  • A and 2SM-5 type zeoli tic crystal films were synthesized on porous supports from the reaction mixture of 1.9 ${SiO}_2$1.5 $Na_20-Al_2O_3-40$ $H_20$ and $Si0_2$-0.l3 $Na_2O$-52 $H_20$-O.l2 TPAOH composition, respectively. The zeolite films were characterized by XRD and SEM. The 2SM -5 crystals grown on the porous matrix were very closely bound together. It was so difficult to obtain the perfectly intergrown crystals in the case of A-type zeolite and this crystal was transformed into P-type zeolite membrane with a prolonged reaction time. The densely intergrown A type zeolite crystal membrane could be also synthesized by the hydrothermal treatment at 100$^{\cirt}C$ after pressing the reaction mixture without addition of water. The pervaporation performance of the synthesized porous inorganic membranes was investigated for alcohol and water mixtures. A-type zeolite membrane crystallized as a thin film showed the selective \'Jermeability of water from the mixtures through the molecular sieving activity of micropores.

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Particle Shapes and Optical Property of Synthesized ZnO with Amine Additives (아민첨가제를 사용하여 합성된 ZnO의 입자형상 및 광학적 특성)

  • Hyeon, Hye-Hyeon;Hyun, Mi-Ho;Lee, Dong-Kyu
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.1
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    • pp.23-29
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    • 2016
  • Zinc oxide of hexagonal wurzite, is known as n-type semiconductor. It has a wide band gap energy of 3.37 eV and large exciton binding energy of 60 meV. It can be widely applied to gas sensors, laser diodes, dye-sensitized solar cells and degradation of dye waste. The use of microwave hydrothermal synthesis brings a rapid reaction rate, high yield, and energy saving. Amine additives control the different particle shapes because of the chelate effect and formation of hydroxide ion. In this study, zinc nitrate hexahydrate was used as zinc precursor. In addition, ethanolamine, ethylenediamine, diethylenetriamine, and hexamethylenetetramine are used as shape control agent. The pH value was controlled as 11 by NaOH. The shapes of zinc oxide are star-like, rod, flower-like, and circular cone. In order to analyze physical, chemical, and optical properties of ZnO with diverse amine additives, we used XRD, SEM, EDS, FT-IR, UV-Vis spectroscopy, and PL spectroscopy.

Green synthesis of fluorescent carbon dots from carrot juice for in vitro cellular imaging

  • Liu, Yang;Liu, Yanan;Park, Mira;Park, Soo-Jin;Zhang, Yifan;Akanda, Md Rashedunnabi;Park, Byung-Yong;Kim, Hak Yong
    • Carbon letters
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    • v.21
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    • pp.61-67
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    • 2017
  • We report the use of carrot, a new and inexpensive biomaterial source, for preparing high quality carbon dots (CDs) instead of semi-conductive quantum dots for bioimaging application. The as-derived CDs possessing down and up-conversion photoluminescence features were obtained from carrot juice by commonly used hydrothermal treatment. The corresponding physiochemical and optical properties were investigated by electron microscopy, fluorescent spectrometry, and other spectroscopic methods. The surfaces of obtained CDs were highly covered with hydroxyl groups and nitrogen groups without further modification. The quantum yield of as-obtained CDs was as high as 5.16%. The cell viability of HaCaT cells against a purified CD aqueous solution was higher than 85% even at higher concentration ($700{\mu}g\;mL^{-1}$) after 24 h incubation. Finally, CD cultured cells exhibited distinguished blue, green, and red colors, respectively, during in vitro imaging when excited by three wavelength lasers under a confocal microscope. Offering excellent optical properties, biocompatibility, low cytotoxicity, and good cellular imaging capability, the carrot juice derived CDs are a promising candidate for biomedical applications.

Aldol Condensation over Acid-Base Bifunctional Metal-Organic Framework Catalysts (산, 염기 이원기능 금속-유기 구조체 촉매를 이용한 알돌 축합반응)

  • Chung, Young-Min
    • Clean Technology
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    • v.20 no.2
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    • pp.116-122
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    • 2014
  • Various types of MOFs (metal-organic frameworks) were prepared via hydrothermal and post-grafting methods and applied as catalysts for the synthesis of jasminaldehyde, one of the representative perfume intermediates, by Aldol condensation of benzaldehyde with heptanal. Although both acid and base sites could catalyze the reaction, the catalytic performance was strongly dependent on the physical properties as well as the nature of functionalization on MOFs. While the use of sulfonated MOF catalysts led to decrease of jasminaldehyde selectivity regardless of MOFs used, the selectivity change was found to rely on the MOF types in the case of the amine-functionalization. Among the catalysts tested, MIL-101 shows the best catalytic performance, which may suggest that MIL-101 has suitable acid properties to promote the Aldol condensation and the large pore of MIL-101 is also advantageous to alleviate the diffusion problem of bulky products.

Properties of Zeolite Nanopowder Coated with Titanium Dioxide by Atomic Layer Deposition

  • Lee, Bo Kyung;Ok, Hae Ryul;Bae, Hye Jin;Kim, Hyug Jong;Choi, Byung Ho
    • Korean Journal of Materials Research
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    • v.26 no.3
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    • pp.149-153
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    • 2016
  • Nanosized zeolites were prepared in an autoclave using tetraethoxysilane (TEOS), tetrapropylammonium hydroxide (TPAOH), and $H_2O$, at various hydrothermal synthesis temperatures. Using transmission electron microscopy and particle size analysis, the nanopowder particulate sizes were revealed to be 10-300 nm. X-ray diffraction analysis confirmed that the synthesized nanopowder was silicalite-1 zeolite. Using atomic layer deposition, the fabricated zeolite nanopowder particles were coated with nanoscale $TiO_2$ films. The $TiO_2$ films were prepared at $300^{\circ}C$ by using $Ti[N(CH_3)_2]_4$ and $H_2O$ as precursor and reactant gas, respectively. In the TEM analysis, the growth rate was ${\sim}0.7{\AA}/cycle$. Zeta potential and sedimentation test results indicated that, owing to the electrostatic repulsion between $TiO_2$-coated layers on the surface of the zeolite nanoparticles, the dispersibility of the coated nanoparticles was higher than that of the uncoated nanoparticles. In addition, the effect of the coated nanoparticles on the photodecomposition was studied for the irradiation time of 240 min; the concentration of methylene blue was found to decrease to 48%.

Synthesis and Characterization of MoS2/Graphene-TiO2 Ternary Photocatalysts for High-Efficiency Hydrogen Production under Visible Light

  • Zhang, Feng-Jun;Kong, Cui;Li, Xuan;Sun, Xian-Yang;Xie, Wen-Jie;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.56 no.3
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    • pp.284-290
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    • 2019
  • Ternary MoS2/graphene (G)-TiO2 photocatalysts were prepared by a simple hydrothermal method. The morphology, phase structure, band gap, and catalytic properties of the prepared samples were investigated by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, UV-vis spectrophotometry, and Brunauer-Emmett-Teller surface area measurement. The H2 production efficiency of the prepared catalysts was tested in methanol-water mixture under visible light. MoS2/G-TiO2 exhibited the highest activity for photocatalytic H2 production. For 5 wt.% and 1 wt.% MoS2 and graphene (5MT-1G), the production rate of H2 was as high as 1989 µmol-1h-1. The catalyst 5MT-1G showed H2 production activity that was ~ 11.3, 5.6, and 4.1 times higher than those of pure TiO2, 1GT, and 5MT, respectively. The unique structure and morphology of the MoS2/G-TiO2 photocatalyst contributed to its improved hydrogen production efficiency under visible light.

Controlled Synthesis of FeSe2 Nanoflakes Toward Advanced Sodium Storage Behavior Integrated with Ether-Based Electrolyte

  • Chen, Yalan;Zhang, Jingtong;Liu, Haijun;Wang, Zhaojie
    • Nano
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    • v.13 no.12
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    • pp.1850141.1-1850141.11
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    • 2018
  • Sodium ion batteries based on the more sodium source reserve than that of lithium have been designed as promising alternatives to lithium ion batteries. However, several problems including unsatisfied specific capacity and serious cyclic stability must be solved before the reality. One of the effective approaches to solve the abovementioned problems is to search for suitable anode materials. In this work, we designed and prepared $FeSe_2$ nanoflakes via a simple hydrothermal method which can be adjusted in composition by Fe precursor. As a potential anode for sodium storage, the optimized $FeSe_2$ electrode was further evaluated in different electrolytes of $NaClO_4$ in propylene carbonate/fluoroethylene carbonate and $NaCF_3SO_3$ in diethylene glycol dimethyl ether. The capacity was about $470mAh\;g^{-1}$ and $535mAh\;g^{-1}$ at $0.5A\;g^{-1}$, respectively, in the voltage between 0.5 V and 2.9 V in the cycle of stabilization phase. Superior performance both in capacity and in stability was obtained in ether-based electrolyte, which affords the property without plugging the intermediates of transition metal dichalcogenides during charge/discharge processes.

Fabrication and Photoelectrochemical Properties of an Oxide Photoanode with Zinc Oxide Nanorod Array Embedded in Cuprous Oxide Thin Film (산화아연 나노막대가 내장된 아산화구리 박막 구조를 이용한 산화물 광양극 제작 및 광전기화학적 특성)

  • Min, Byeongguk;Kim, Hyojin
    • Korean Journal of Materials Research
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    • v.29 no.3
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    • pp.196-203
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    • 2019
  • We report on the fabrication and characterization of an oxide photoanode with a zinc oxide (ZnO) nanorod array embedded in cuprous oxide ($Cu_2O$) thin film, namely a $ZnO/Cu_2O$ oxide p-n heterostructure photoanode, for enhanced efficiency of visible light driven photoelectrochemical (PEC) water splitting. A vertically oriented n-type ZnO nanorod array is first prepared on an indium-tin-oxide-coated glass substrate via a seed-mediated hydrothermal synthesis method and then a p-type $Cu_2O$ thin film is directly electrodeposited onto the vertically oriented ZnO nanorod array to form an oxide p-n heterostructure. The introduction of $Cu_2O$ layer produces a noticeable enhancement in the visible light absorption. From the observed PEC current density versus voltage (J-V) behavior under visible light illumination, the photoconversion efficiency of this $ZnO/Cu_2O$ p-n heterostructure photoanode is found to reach 0.39 %, which is seven times that of a pristine ZnO nanorod photoanode. In particular, a significant PEC performance is observed even at an applied bias of 0 V vs $Hg/Hg_2Cl_2$, which makes the device self-powered. The observed improvement in the PEC performance is attributed to some synergistic effect of the p-n bilayer heterostructure on the formation of a built-in potential including the light absorption and separation processes of photoinduced charge carriers, which provides a new avenue for preparing efficient photoanodes for PEC water splitting.