• Title/Summary/Keyword: Hydrothermal reaction

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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.

Syntheses of FAPO-5 Molecular Sieves with Microwave Irradiation and Their Characterization (마이크로파 가열에 의한 FAPO-5 분자체의 합성 및 특성 분석)

  • Jang, Jong-San;Lee, Jin-Ho;Jeong, Seong-Hwa;Hwang, Jin-Su
    • Journal of the Korean Chemical Society
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    • v.50 no.1
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    • pp.53-59
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    • 2006
  • .FAPO-5 molecular sieves were synthesized starting from the same reactant gel at 170 oC using microwave irradiation technique and conventional hydrothermal reaction. The FAPO-5 molecular sieves were characterized by several techniques such as SEM, FTIR, UV/Vis, and ESR. Moreover, the oxidation of styrene over FAPO-5s was carried out, and compared to check the oxidation and epoxidation ability of the two FAPO-5s. FAPO-5 can be obtained easily by microwave irradiation within 15 min at 170oC, whereas FAPO-5 synthesis is completed in 6 h by conventional electric heating, confirming the acceleration about 20 times by microwave technique. There are no appreciable differences between two FAPO-5s in surface area and coordination state of iron. The FAPO-5 synthesized by microwave irradiation shows higher epoxide selectivity in the styrene epoxidation, which may be explained by the higher hydrophobicity of the catalyst.

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.

Electrochemical Characteristics of Synthesized Nb2O5-Li3VO4 Composites as Li Storage Materials

  • Yang, Youngmo;Seo, Hyungeun;Kim, Jae-Hun
    • Corrosion Science and Technology
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    • v.20 no.4
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    • pp.183-188
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    • 2021
  • The increasing demand for energy storage in mobile electronic devices and electric vehicles has emphasized the importance of electrochemical energy storage devices such as Li-ion batteries (LIBs) and supercapacitors. For reversible Li storage, alternative anode materials are actively being developed. In this study, we designed and fabricated an Nb2O5-Li3VO4 composite for use as an anode material in LIBs and hybrid supercapacitors. Nb2O5 powders were dissolved into a solution and the precursors were precipitated onto Li3VO4 through a simple, low-temperature hydrothermal reaction. The annealing process yielded an Nb2O5-Li3VO4 composite that was characterized by X-ray diffraction, electron microscopy, and X-ray photoelectron spectroscopy. Electrochemical tests revealed that the Nb2O5-Li3VO4 composite electrode demonstrated increased capacities of approximately 350 and 140 mAh g-1 at 0.1 and 5 C, respectively, were maintained up to 1000 cycles. The reversible capacity and rate capability of the composite electrode were enhanced compared to those of pure Nb2O5-based electrodes. These results can be attributed to the microstructure design of the synthesized composite material.

Photocatalytic Generated Oxygen Species Properties by Fullerene Modified Two-Dimensional MoS2 and Degradation of Ammonia Under Visible Light

  • Zou, Cong-Yang;Meng, Ze-Da;Zhao, Wei;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.31 no.6
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    • pp.353-366
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    • 2021
  • In this study, photocatalytic degradation of ammonia in petrochemical wastewater is investigated by solar light photocatalysis. Two-dimensional ultra-thin atomic layer structured MoS2 are synthesized via a simple hydrothermal method. We examine all prepared samples by means of physical techniques, such as SEM-EDX, HRTEM, FT-IR, BET, XRD, XPS, DRS and PL. And, we use fullerene modified MoS2 nanosheets to enhance the activity of photochemically generated oxygen (PGO) species. Surface area and pore volumes of the MoS2-fullerene samples significantly increase due to the existence of MoS2. And, PGO oxidation of MB, TBA and TMST, causing its concentration in aqueous solution to decrease, is confirmed by the results of PL. The generation of reactive oxygen species is detected through the oxidation reaction from 1,5-diphenyl carbazide (DPCI) to 1,5-diphenyl carbazone (DPCO). It is found that the photocurrent density and the PGO effect increase in the case with modified fullerene. The experimental results show that this heterogeneous catalyst has a degradation of 88.43% achieved through visible light irradiation. The product for the degradation of NH3 is identified as N2, but not NO2- or NO3-.

Au-Ag-Te Mineralization by Boiling and Dilution of Meteoric Ground-water in the Tongyeong Epithermal sold System, Korea: Implications from Reaction Path Modeling (광화유체의 비등과 희석에 의한 통영 천열수계 Au-Ag-Te 장화작용에 대한 반응경로 모델링)

  • Maeng-Eon Park;Kyu-Youl Sung
    • Economic and Environmental Geology
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    • v.34 no.6
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    • pp.507-522
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    • 2001
  • At the Tongyeong mine, quartz, rhodochrosite (kutnahorite), muscovite, illite, pyrite, galena, chalcopyrite. sphalerite, acanthite, and hessite are the principal vein minerals. They were deposited under epithermal conditions in two stages. Ore mineral assemblages and associated gangue phases in stage can be clearly divided into two general associations: an early cycle (band) that appeared with introduction of most of the sulfides and electrum, and a later cycle in which base metal and carbonate-bearing assemblages (mostly rhodochrosite) became dominant. Tellurides and some electrum occur as small rounded grains within subhedral-to euhedral pyrite or anhedral galena in stageII. Sulfide mineralization is zoned from pyrite to galena and sphalerite. We have used computer modeling to simulate formation of four stages of vein genesis. The reaction of a single fluid with andesite host rock at 28$0^{\circ}C$, isobaric cooling of a single fluid from 26$0^{\circ}C$ to 12$0^{\circ}C$, and boiling and mixing of a fluid with both decreasing pressure and temperature were studied using the CHILLER program. Calculations show that the precipitation of alteration minerals is due to fluid-andesite interaction as temperature drops. Speciation calculations confirm that the hydrothermal fluids with moderately high salinities and pH 5.7 (acid), were capable of transporting significant quantities of base metals. The abundance of gold in fluid depends critically on the ratio of total base metals and iron to sulfide in the aqueous phase because gold is transported as an Au(HS)$_2$- complex, which is sensitive to sulfide activity. Modeling results for Tongyeong mineralization show strong influence of shallow hydrogenic processes such as boiling and fluid mixing. The variable handing in stageII mineralization is best explained by maltiple boilings of hydrothermal fluid followed by lateral mixing of the fluid with overlying diluted, steam-heated ground water. The degree of similarity of calculated mineral assemblages and observed electrum composition and field relationships shows the utility of the numerical simulation method in identifying chemical processes that accompany boiling and mixing in Te-bearing Au-Ag system. This has been applied in models to narrow the search area for epithermal ores.

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Scaling up Hydrothermal Synthesis of Na-A Type Zeolite from Natural Siliceous Mudstone and Its Heavy Metal Adsorption Behavior (규질 이암으로부터 Na-A형 제올라이트의 scale-up 수열합성 및 중금속흡착)

  • Bae, In-Kook;Jang, Young-Nam;Shin, Hee-Young;Chae, Soo-Chun;Ryu, Kyoung-Won
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.4
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    • pp.341-347
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    • 2008
  • The feasibility of commercializing the hydrothermal synthesis of Na-A type zeolite from siliceous mudstone has been conducted using a 50-liter bench-scale autoclave and the application of the zeolite as an environmental remediation agent. Siliceous mudstone, which is widely distributed around the Pohang area, was adopted as a precursor. The siliceous mudstone is favorable for the synthesis of zeolite because it contains 70.7% $SiO_2$ and 10.0% $Al_2O_3$, which are major ingredient of zeolite formation. The synthesis of zeolite was carried out under the following conditions that had been obtained from the previous laboratory-scale tests: 10hr reaction time, $80^{\circ}C$ reaction temperature, $Na_2O/SiO_2$ ratio = 0.6, $SiO_2/Al_2O_3$ ratio = 2.0 and $H_2O/Na_2O$ ratio= 98.6. The crystallinity and morphology of the zeolite formed were similar to those obtained from the laboratory-scale tests. The recovery and cation exchange ion capacity were 95% and 215 cmol/kg, respectively, which are slightly higher than those obtained in laboratory scale tests. To examine the feasibility of the zeolite as an environmental remediation agent, experiments for heavy metal adsorption to zeolite were conducted. Its removal efficiencies of heavy metals in simulated waste solutions decreased in the following sequences: Pb > Cd > Cu = Zn > Mn. In a solution of 1500 mg/L total impurity metals, the removal efficiencies for these impurity metals were near completion (> 99%) except for Mn whose efficiency was 98%. Therefore, the synthetic Na-A type zeolite was proven to be a strong absorbent effective for removing heavy metals.

Anode Properties of TiO2 Nanotube for Lithium-Ion Batteries (리튬이온전지용 TiO2 나노튜브 음전극 특성)

  • Choi, Min Gyu;Lee, Young-Gi;Kim, Kwang Man
    • Korean Chemical Engineering Research
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    • v.48 no.3
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    • pp.283-291
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    • 2010
  • In this review, the studies on the electrochemical properties of $TiO_2$ nanotube as an anode material of lithium-ion battery, which was prepared by an alkaline hydrothermal reaction and anneling process, were investigated andanalyzed in terms of charge-dischage characteristics. Up to date, a maximum discharge capacity of $338mAh\;g^{-1}$(x=1.01) was achieved by the nanotube with $TiO_2(B)$ phase, whereas the theoretical capacity of $TiO_2$ anode was $335mAh\;g^{-1}$(x=1) in the basis of $Li_xTiO_2$ as a product of electrochemical reaction between $TiO_2$ and lithium. This was due to fast lithium transport by a shortened diffusion path provided by controlling the nanostructure of $TiO_2$, because the self-diffusion of lithium was slow in a basis of its activation energy as 0.48 eV. Due to an excellent ion storage capabilities in both the surface and the bulk phase, the $TiO_2$ nanotube could be a promising active material as both an anode of lithium-ion battery and an electrode of capacitor with high-rate performances.

CdS-Titania-Nanotube Composite Films for Photocatalytic Hydrogen Production (CdS/Titania-나노튜브 복합 막을 이용한 광촉매적 수소제조)

  • Lee, Hyun-Mi;So, Won-Wook;Baeg, Jin-Ook;Kong, Ki-Jeong;Moon, Sang-Jin
    • Transactions of the Korean hydrogen and new energy society
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    • v.18 no.3
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    • pp.230-237
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    • 2007
  • Titania nanotube(TiNT) and CdS sol were synthesized by hydrothermal reaction under strongly basic condition and by precipitation reaction of $Cd(N0_3)_2$ and $Na_2S$ aqueous solutions, respectively. After preparing a series of CdS-TiNT composite films on $F:SnO_2$ conducting glass with variation of the mole ratio (r) of TiNT/(CdS+TiNT), their visible light absorption, photocatalytic activities for hydrogen production, and the photocurrent generation were examined. In general, this CdS-TiNT series showed lower photocatalytic activities and photocurrent generation under Xe light irradiation compared to their counterparts, i.e., CdS-$TiO_2$ particulate series. It appeared that TiNTs are not so effective photocatalyic material in spite of their larger specific surface areas compared to $TiO_2$ nanoparticles, because they indicate a poor crystallinity and less intimate interaction or contact with CdS particles owing to the tubular morphology and an easy agglomeration among themselves.

A Study on the Fabrication of Lithium Iron Oxide Electrode and its Cyclic Voltammetric Characteristics (리튬-철 산화물 전극의 제조 및 전류전위 순환 특성에 관한 연구)

  • Jeong Won-Joong;Ju Jeh-Beck;Sohn Tai-Won
    • Journal of the Korean Electrochemical Society
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    • v.2 no.3
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    • pp.156-162
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    • 1999
  • Various types of iron oxide based materials as a cathode of lithium secondary battery have been prepared and their electrochemical characteristics have been also observed. In order to understand the fundamental characteristics of iron oxide electrode, three kinds of iron oxides such as iron oxides formed by direct oxidation of iron plate or iron powders and FeOOH powders were tested with cyclic voltammetry. The oxidation and reduction peaks due to the reaction of intercalation and deintercalation were not observed for the iron oxide prepared with iron plate and FeOOH powders. In case of iron oxide prepared from iron powders, only one reduction peak was observed. A layered form of $LiFeO_2$ was synthesized directly from $FeCl_3\cdot6H_2O,\;NaOH\;and\;LiOH$ and LiOH by hydrothermal reaction. The effect of NaOH on the electrode performance was examined. When increasing NaOH, it provides the electrode with less discharge capacity and efficiency, however, decreasing rate of discharge capacity became smaller. $LiFeO_2$ synthesized with the molar ratio of $NaOH/FeCl_3/LiOH$, 2/1/7 showed the largest capacity, but the discharging efficiency was sharply decreased after 30 cycles.