• Title/Summary/Keyword: 수열반응

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Fabrication of Mono-Dispersed Ultrafine BaTiO$_3$ Powder Using Microwave (마이크로파를 이용한 초미세 균일 분산 BaTiO$_3$ 분말 제조)

  • 김현상;최광진;이상균;김영대;심상준;우경자;김경림;조영상
    • Journal of the Korean Ceramic Society
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    • v.36 no.4
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    • pp.343-353
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    • 1999
  • Microwave(2.45 GHz) was used as energy source in hydrothermal reaction to fabricate ultrafine BaTiO3 powder. Using microwave of 700 W, crytal BaTiO3 began to fom after 5 min in microwave-autoclave sys-tem. The crystallinity was not noticeably increased with increasing longer reaction time than 10 min. On the other hand in microwave-reflux system crytal BaTiO3 began to form after 15min and the crystallinity was not noticeably increased with increasing longer reaction time than 1hr,. In either case particle size dis-tribution was considerably uniform due to the effect of homogeneous heating by microwave. In addition mi-crowave heating gave an extremely small degree of particle agglomeration compared to electric heating. Av-erage sizes of as-synthesized powders were 30-60nm. Ba/Ti ratio in sol played an important role in det-ermining the particle size. It seems that excess barium forms different phases such as Ba(OH)2 which makes thin layer on the surface of BaTiO3 powder. This thin layer would inhibit the agglomeration of Ba-TiO3 powders and keep the small grain size. In microwave-autoclave system tetragonal-BaTiO3 was formed directly by the reaction of only 15 min. In the case of microwave-reflux system tetragonal-BaTiO3 was formed by driyng over 25$0^{\circ}C$.

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Photocatalytic Decomposition of Rhodamine B over BiVO4 Doped with Samarium Ion (Sm 이온이 도핑된 BiVO4에서 로다민 B의 광촉매 분해 반응)

  • Hong, Seong-Soo
    • Clean Technology
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    • v.27 no.2
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    • pp.146-151
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    • 2021
  • Pure and Sm ion doped BiVO4 catalysts were synthesized using a conventional hydrothermal method and characterized by XRD, DRS, SEM, and PL. We also examined the activity of these materials on the photocatalytic decomposition of rhodamine B under visible light irradiation. The doping of Sm ion into BiVO4 catalyst changed the ms-BiVO4 crystal structure into the tz-BiVO4 crystal structure in the low synthesis temperature. Light absorption analysis using DRS showed that all the catalysts displayed strong absorption in the visible range of the electromagnetic spectrum regardless of Sm ion doping. In addition, an amorphous morphology was shown in the pure BiVO4 catalyst, but the morphology of the BiVO4 catalyst doped with Sm ion was changed into an ellipse shape and also the particle size decreased. In the photocatalytic decomposition of rhodamine B, Sm ion doped BiVO4 catalyst showed higher photocatalytic activity than the pure BiVO4 catalyst. In addition, the Sm3-BVO catalyst doped with 3% Sm ion showed the highest photocatalytic activity, as well as the highest formation rate of OH radicals (•OH) and the highest PL peak. This result suggests that the formation rate of OH radicals produced in the interface between the photocatalyst and water is well correlated with the photocatalytic activity.

Catalytic CO2 Methanation over Ni Catalyst Supported on Metal-Ceramic Core-Shell Microstructures (금속-세라믹 코어-쉘 복합체에 담지된 Ni 금속 촉매를 적용한 CO2 메탄화 반응 특성연구)

  • Lee, Hyunju;Han, Dohyun;Lee, Doohwan
    • Clean Technology
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    • v.28 no.2
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    • pp.154-162
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    • 2022
  • Microstructured Al@Al2O3 and Al@Ni-Al LDH (LDH = layered double hydroxide) core-shell metal-ceramic composites are prepared by hydrothermal reactions of aluminum (Al) metal substrates. Controlled hydrothermal reactions of Al metal substrates induce the hydrothermal dissolution of Al ions at the Al-substrate/solution interface and reconstruction as porous metal-hydroxides on the Al substrate, thereby constructing unique metal-ceramic core-shell composite structures. The morphology, composition, and crystal structure of the core-shell composites are affected largely by the ions in the hydrothermal solution; therefore, the critical physicochemical and surface properties of these unique metal-ceramic core-shell microstructures can be modulated effectively by varying the solution composition. A Ni/Al@Al2O3 catalyst with highly dispersed catalytic Ni nanoparticles on an Al@Al2O3 core-shell substrate was prepared by a controlled reduction of an Al@Ni-Al LDH core-shell prepared by hydrothermal reactions of Al in nickel nitrate solution. The reduction of Al@Ni-Al LDH leads to the exolution of Ni ions from the LDH shell, thereby constructing the Ni nanoparticles dispersed on the Al@Al2O3. The catalytic properties of the Ni/Al@Al2O3 catalyst were investigated for CO2 methanation reactions. The Ni/Al@Al2O3 catalyst exhibited 2 times greater CO2 conversion than a Ni/Al2O3 catalyst prepared by conventional incipient wetness impregnation and showed high structural stability. These results demonstrate the high effectiveness of the design and synthesis methods for the metal-ceramic composite catalysts derived by hydrothermal reactions of Al metal substrates.

Synthesis of Fe-doped β-Ni(OH)2 microcrystals and their oxygen evolution reactions (Fe 도핑된 β-Ni(OH)2 마이크로결정 합성과 산소발생반응 특성)

  • Je Hong Park;Si Beom Yu;Seungwon Jeong;Byeong Jun Kim;Kang Min Kim;Jeong Ho Ryu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.33 no.5
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    • pp.196-201
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    • 2023
  • In order to improve the efficiency of the water splitting system for hydrogen energy production, the high overvoltage in the electrochemical reaction caused by the catalyst in the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) must be reduced. Among them, transition metal-based compounds (hydroxide, sulfide, etc.) are attracting attention as catalyst materials to replace currently used precious metals such as platinum. In this study, Ni foam, an inexpensive metal porous material, was used as a support and β-Ni(OH)2 microcrystals were synthesized through a hydrothermal synthesis process. In addition, changes in the crystal morphology, crystal structure, and water splitting characteristics of β-Ni(OH)2 microcrystals synthesized by doping Fe to improve electrochemical properties were observed, and applicability as a catalyst in a commercial water electrolysis system was examined.

Effects of Mo co-doping into Fe doped β-Ni(OH)2 microcrystals for oxygen evolution reactions (Fe-doped β-Ni(OH)2의 산소발생반응 증가를 위한 Mo의 동시도핑효과)

  • Je Hong Park;Si Beom Yu;Tae Kwang An;Byeong Jun Kim;Jeong Ho Ryu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.34 no.1
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    • pp.30-35
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    • 2024
  • In order to improve the efficiency of the water splitting system for hydrogen production, the high overvoltage in the electrochemical reaction caused by the catalyst in the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) must be reduced. Among them, transition metal-based compounds are attracting attention as catalyst materials that can replace precious metals such as platinum that are currently used. In this study, nickel foam, an inexpensive metal porous material, was used as a support, and Fe-doped β-Ni(OH)2 microcrystals were synthesized through a hydrothermal synthesis process. In addition, in order to improve OER properties, changes in the shape, crystal structure, and water splitting characteristics of Fe-Mo co-doped β-Ni(OH)2 microcrystals synthesized by co-doping with Mo were observed. The changes in the shape, crystal structure, and applicability as a catalyst for water splitting were examined.

Preparation and Characterization of $Cu/Ce_xZr_{1-x}O_2$ Catalysts for Preferential Oxidation of Carbon Monoxide (일산화탄소의 선택적 산화반응을 위한 $Cu/Ce_xZr_{1-x}O_2$ 촉매의 합성과 특성분석)

  • Lee, So-Yeon;Lee, Suk-Hee;Cheon, Jae-Kee;Woo, Hee-Chul
    • Clean Technology
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    • v.13 no.1 s.36
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    • pp.54-63
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    • 2007
  • Even traces of CO in the hydrogen-rich feed gas to proton exchange membrane fuel cells (PEMFC) poison the platinum anode electrode and dramatically decrease the power output. In this work, a variety of catalytic materials consisting of $Cu/Ce_xZr_{1-x}O_2$, (x = 0.0-1.0) were synthesised, characterized and tested for CO oxidation and preferential oxidation of CO (PROX). These catalysts prepared by hydrothermal and deposition-precipitation methods. The catalysts were characterized by XRD, XRF, SEM, BET, $N_2O$ titration and oxygen storage capacity (OSC) measurement. The effects of composition of the support and degree of excess oxygen were investigated fur activity and $CO_2$ selectivity with different temperatures. The composition of the support markedly influenced the PROX activity. Among the various $Cu/Ce_xZr_{1-x}O_2$ catalysts having different composition, $Cu/Ce_{0.9}Zr_{0.1}O_2$ and $Cu/Ce_{0.7}Zr_{0.3}O_2$ showed the highest activities (>99%) and selectivities (ca.50%) in the temperature range of $150{\sim}160^{\circ}C$. It was found that by using of $Ce_xZr_{1-x}O_2$ mixed oxide support which possesses a high oxygen storage capacity, oxidation-reduction activity of Cu-based catalyst was improved, which resulted in the increase of catalytic activity and selectivity of CO oxidation in excess $H_2$ environments.

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Characterization of manganese oxide supercapacitors using carbon cloth (Carbon Cloth을 이용한 이산화망간 슈퍼커패시터 특성 연구)

  • Lee, Seung Jin;Kim, Chihoon;Ji, Taeksoo
    • Journal of Digital Contents Society
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    • v.18 no.6
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    • pp.1199-1205
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    • 2017
  • Global energy consumption is rapidly increasing yearly due to drastic industrial advances, requiring the development of new energy storage devices. For this reason, supercapacitors with fast charge-discharge, long life cycle and high power density is getting attention, and have been considered as one of the potential energy storage systems. In this research, we developed a supercapacitor that consists of amorphous manganese oxide($MnO_2$) electrodes deposited onto carbon cloth substrates using the hydrothermal method. The Fe-doped amorphous $MnO_2$ samples were characterized by X-ray diffraction(XRD), Energy Dispersive X-ray spectroscopy(EDX), as well as scanning electron microscopy(SEM). The electrochemical analysis of the prepared samples were performed using cyclic voltammetry and galvanostatic charge-discharge measurements in 1M $Na_2SO_4$ electrolyte. The test results demonstrate that the supercapacitor based on the Fe-doped amorphous $MnO_2$ electrodes has a specific capacitance as high as 163F/g at 1A/g current density, and good cycling stability of 87.34% capacitance retention up to 1000 cycles.

Synthesis of PbMo1-xCrxO4 Oxides Prepared Using Hydrothermal Process and their Photocatalytic Activity (수열합성법에 의한 PbMo1-xCrxO4 산화물의 합성 및 광촉매 활성)

  • Song, Young In;Hong, Seong-Soo
    • Applied Chemistry for Engineering
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    • v.26 no.6
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    • pp.714-718
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    • 2015
  • Both lead molybdate ($PbMoO_4$) and chromium substituted lead molybdate ($PbMo_{1-x}Cr_xO_4$) were successfully synthesized using a conventional hydrothermal method and characterized by XRD, DRS, Raman, SEM and PL. We also investigated the photocatalytic activity of these materials for the decomposition of rhodamine B under UV-visible irradiation. The XRD and Raman results revealed the successful synthesis of well-crystallized $PbMoO_4$ crystals with the diameter of 51-59 nm, regardless of the addition of chromium ion. The DRS spectra of $PbMo_{1-x}Cr_xO_4$ catalysts showed new intensive absorption bands in the visible region. The $PbMoO_4$ catalysts showed the lowest photocatalytic activity and the activity increased with an increase of chromium substitution amounts under visible irradiation. PL peaks appeared at about 540-580 nm for all catalysts and excitonic PL signals were proportional to the photocatalytic activity for the decomposition of rhodamine B.

Hydrothermal Synthesis and Transition Metal Cations Exchange Characterization of Titanium and [Titanium+Alkali Metals] Substituted-11Å Tobermorites

  • El-Korashy, S.A.
    • Journal of the Korean Chemical Society
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    • v.48 no.2
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    • pp.129-136
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    • 2004
  • Titanium and [titanium+Na(K)] substituted 11${\AA}$ tobermorites solids synthesized under hydrothermal conditions at 180$^{\circ}C$ exhibit cation exchange properties toward heavy transition metal cations, such as Fe$^{2+},\;Zn^{2+},\;Cd^{2+}\;and/or\;Pb^{2+}$. The amount of heavy metal cations taken up by these solids was found in the order: Fe$^{2+}>Zn^{2+}>Cd^{2+}>Pb^{2+}$, and reached maximum at 10% [Ti+K]-substituted tobermorite. The total cation exchange capacity of the 10% Ti+Na (K) - substituted tobermorites synthesized here range from 71 to 89 meq/100 g, and 50-56 meq/100g for Ti-substituted only. Results indicated that 10% [Ti+K] substitution exhibit cation exchange capacity more 2.4 times than the unsubstituted-tobermorite. This is due to the increase of the number of active sites on the exchangers. The incorporation of Ti and/or [Ti+Na(K)] in the lattice structure of synthesized tobermorites is due to exchange of Ti$^{4+}{\Leftrightarrow}2Ca^{2+}\;and/or\;Ti^{4+}+2Na^+(K^+){\Leftrightarrow}3Ca^{2+}$, respectively. The mechanism of Ti and [Ti+Na(K)] incorporations in the crystal lattice of the solids during synthesis and the heavy metal cations uptaken by these solids is studied.

Hydrothermal Synthesis of Li-Mn Spinel Nanoparticle from K-Birnessite and Its Electrochemical Characteristics (K-Birnessite를 이용한 Li-Mn Spinel 나노입자 합성 및 전기화학적 특성 평가)

  • Kim, Jun-Il;Lee, Jae-Won;Park, Sun-Min;Roh, Kwang-Chul;Sun, Yang-Kook
    • Applied Chemistry for Engineering
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    • v.21 no.5
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    • pp.590-592
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    • 2010
  • Li-Mn spinel ($LiMn_2O_4$) is prepared by a hydrothermal process with K-Birnessite ($KMnO_4{\cdot}yH_2O$) as a precursor. The K-Birnessite obtained via a hydrothermal process with potassium permanganate [$KMnO_4$] and urea [$CO(NH_2)_2$] as starting materials are converted to Li-Mn spinel nanoparticles reacting with LiOH. The molar ratio of LiOH/K-Birnessite is adjusted in order to find the effect of the ratio on the structural, morphological and electrochemical performances of the Li-Mn spinel. X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and thermogravimetry (TG) are used to investigate the crystal structure and morphology of the samples. Galvanostatic charge and discharge are carried out to measure the capacity and rate capability of the Li-Mn spinel. The capacity shows a maximum value of $117\;mAhg^{-1}$ when the molar ratio of LiOH/K-Birnessite is 0.8 and decreases with the increase of the ratio. However the rate capability is improved with the increase of the ratio due to the reduction of the particle size.