• 제목/요약/키워드: Hydrothermal synthesis methods

검색결과 37건 처리시간 0.031초

수열합성법으로 합성된 산화아연 나노 구조 박막의 광촉매적 응용 (Hydrothermally Synthesis Nanostructure ZnO Thin Film for Photocatalysis Application)

  • ;남민식;;전성찬
    • KEPCO Journal on Electric Power and Energy
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    • 제2권1호
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    • pp.97-101
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    • 2016
  • 산화아연은 다양한 나노 구조와 특유의 특성으로 인하여 여러 분야에서 많은 관심을 받고있는 물질이다. 산화아연을 합성하는 다양한 방법 중에서, 수열합성법은 간단하고 친환경적인 장점을 가지고 있다. 나노 구조를 가지는 산화아연 박막은 수열합성법을 통하여 FTO 전극 위에 제작되었다. 성장된 산화아연은 X-ray diffraction (XRD)와 Field-emission scanning electron microscopy (FESEM)을 통하여 분석되었다. XRD 분석에서 산화아연 박막이 자연상태의 hexagonal wurtzite 상으로 구성되어 있음을 확인하였으며 SEM 사진에서는 나노 로드 형태를 구성하고 있는 것을 확인할 수 있었다. 본 연구에서는 UV 영역의 흡수 스펙트럼을 분석하여 산화아연이 보이는 365 nm 파장에서의 흡수를 확인하였다. 또한 photoluminescence 방출을 분석한 결과, 424 nm의 band edge emission과 500 nm에서 산화아연의 oxygen vacancies에 의한 방출을 확인하였다. 또한 라만 스펙트럼 분석을 통하여 본 연구진이 제작한 산화아연이 높은 결정성을 가지고 있는 것을 확인할 수 있었다. 이러한 연구를 통하여 다양한 특성을 가진 산화아연의 광촉매적 적용을 기대할 수 있다.

Synthesis of Yttria Stabilized Zirconia by Sol-gel Precipitation Using PEG and PVA as Stabilizing Agent

  • Bramhe, Sachin N.;Lee, Young Pil;Nguyen, Tuan Dung;Kim, Taik-Nam
    • 한국재료학회지
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    • 제23권8호
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    • pp.441-446
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    • 2013
  • There is increasing interest in zirconia as a dental material due to its aesthetics, as well as the exceptionally high fracture toughness and high strength that are on offer when it is alloyed with certain oxides like yttria. In recent years, many solution based chemical synthesis methods have been reported for synthesis of zirconia, of which the sol-gel method is considered to be best. Here, we synthesize zirconia by a sol gel assisted precipitation method using either PEG or PVA as a stabilizing agent. Zirconia sol is first synthesized using the hydrothermal method. We used NaOH as the precipitating agent in this method because it is easy to remove from the final solution. Zirconium and yttrium salts are used as precursors and PEG or PVA are used as stabilizers to separate the metal ions. The resulting amorphous zirconia powder is calcined at $900^{\circ}C$ for 2 h to get crystallized zirconia. XRD analysis confirmed the partially stabilized zirconia synthesis in all the synthesized powders. SEM was taken to check the morphology of the powder synthesized using either PEG or PVA as a stabilizing agent and finally the transparency was calculated. The results confirmed that the powder synthesized with 10 % PVA as the stabilizing agent had highest percentage of transparency among all the synthesized powder.

Low Temperature Synthesis of TiO2 Films for Application to Dye-sensitized Solar Cells

  • 위진성;최은창;서영호;홍병유
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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    • pp.475-475
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    • 2014
  • Dye sensitized solar cells (DSSCs) are regarded as potential inexpensive alternatives to conventional solid-state devices. The flexible version, employing conductive-plastic-film substrates, is appealing for commercialization of DSSCs because it not only reduces the weight and cost of the device but also extends their applications. However, the need for high temperature does not permit the use of plastic-film substrate. So, development of low-temperature methods is therefore realization of flexible DSSCs. In this work, the electrophoretic deposition combined with hydrothermal treatment was employed to prepare nanocrystalline $TiO_2$ thin film at low temperature. We confirmed the prepared $TiO_2$ thin films with different voltages and deposition times in the electrophoretic deposition process. Properties of the $TiO_2$ films were investigated by various analysis method such as X-ray diffraction, field emission scanning electron microscopy (FESEM) and UV-visible spectrophotometer.

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수열합성법에 의한(Ni, Zn)-Ferrites의 초미세분말 합성공정 및 $CO_2$분해 특성 연구 (Study on The Synthesis of The Ultra-Fine (Ni, Zn)-ferrite by The Hydrothermal Method and its $CO_2$ Decomposition)

  • 김정식;안정률;류호진
    • 한국재료학회지
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    • 제10권3호
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    • pp.223-226
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    • 2000
  • 산소 결핍 페라이트 (oxygen deficient ferrites, ODF) $MeFe_2O_{4-\delta}$는 약 $300^{\circ}C$의 낮은 온도에서 $CO_2$를 C와 $O_2$로 분해한다. 본 연구에서는 $(Ni_x,\;Zn_{1-x}Fe_2_4$ 초미세 페라이트 분말을 수열합성법으로 제조하여 $CO_2$ 분해특성을 살펴보았다. 제조된 페라이트는 XRD 분석 결과, 페라이트의 전형적인 스피넬 구조를 보여주고 있으며, ICP-AES, EDS 정량분석에 의하여 초기 혼합 조성비와 거의 동일한 조성비로 합성되었음을 알 수 있었다. 제조된 (Ni, Zn)-ferrites 분말의 BET 비표면적은 약 $110\textrm{mg}^2$/g$ 이상의 큰 값으로 나타났으며, 입자크기는 약 5~10nm로 매우 작았다. 산소결핍 페라이트 $(Ni_x,\;Zn_{1-x})Fe_2O_{4-{$\delta}}$$CO_2$ 분해 효율은 조성에 따라 큰 차이를 보이지 않았으며 3원계 (Ni, Zn)-ferrite가 Ni-ferrite보다 더 높았다.

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무기물계 폐기물로 합성한 제올라이트의 코발트, 니켈, 구리 이온의 회수 성능 (The Recovery Performance of Co, Ni, and Cu Ions Using Zeolites Synthesized from Inorganic Solid Wastes)

  • 이창한
    • 한국물환경학회지
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    • 제28권5호
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    • pp.723-728
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    • 2012
  • In this study, zeolites were synthesized by a fusion and a hydrothermal methods using a coal fly ash and a waste catalyst. The recovery performance of metal ions on the structure property of synthetic zeolites was evaluated as comparing the adsorption kinetics (Lagergen 2nd order model) and isotherm (Langmuir model) of $Co^{2+},\;Ni^{2+}$, and $Cu^{2+}$ ions. The synthetic zeolites (Z-C1 and Z-W5) were similarly assigned to XRD peaks in a reagent grade Na-A zeolite (Z-WK : $Na_{12}Al_{12}Si_{12}O_{48}\;27.4H_2O$). Adsorption rates of Z-W5 and Z-C1 were in the order of $Cu^{2+}\;>\;Co^{2+}\;>\;Ni^{2+}\;and\;Ni^{2+}\;>\;Cu^{2+}\;>\;Co^{2+}$, respectively. They had influenced upon structure properties of zeolite. Selectivities of metal ions and maximum equilibrium adsorption capacities, $q_{max}$, in Z-C1 and Z-W5 were in the order of $Ni^{2+}$ (127.9 mg/g) > $Cu^{2+}$ (94.7 mg/g) > $Co^{2+}$ (82.6 mg/g) and $Cu^{2+}$ (141.3 mg/g) > $Co^{2+}$ (122.2 mg/g) > $Ni^{2+}$ (87.6 mg/g), respectively. The results show that the synthetic zeolites, Z-C1 and Z-W5, are able to recover metal ions selectively in wastewater.

Influence of RTA treatments on optical properties of ZnO nanorods synthesized by wet chemical method

  • Shan, Qi;Ko, Y.H.;Lee, H.K.;Yu, J.S.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2009년도 제38회 동계학술대회 초록집
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    • pp.190-190
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    • 2010
  • Zinc oxide is the most attractive material due to the large direct band gap (3.37 eV), excellent chemical and thermal stability, and large exciton binding energy (60 meV). Recently, ZnO nanorods were used as the high efficient antireflection coating layer of solar cells based on silicon (Si). In this reports, we studied the effects of rapid thermal annealing (RTA) treatment on optical properties of ZnO nanorods. For fabrication of ZnO nanorods, there are many methods such as hydrothermal method, sol-gel method, and metal organic chemical vapor deposition method. Among of them, we used the conventional wet chemical method which is simple and low temperature growth. In order to synthesize the ZnO nanorods, the ZnO films were deposited on Si substrate by RF magnetron sputtering at room temperature and the samples were dipped to aqua solution containing the zinc nitrate and hexamethylentetramines (HMT). The synthesis process was achieved in keeping with temperature of $90-95^{\circ}C$ and under constant stirring. The morphology of ZnO nanorods on glass and Si was characterized by scanning electron microscopy. For the analysis of antireflection performance, the reflectance and transmittance were measured by spectrophotometer. And for analyzing the effects of RTA treatment on ZnO nanorods, crystalline properties were investigated by X-ray diffraction measurements and optical properties was estimated by photoluminescence spectra.

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실리카테인: 생규화 및 응용 (Silicatein: Biosilicification and Its Applications)

  • 양병선;윤진영;차형준
    • 한국해양바이오학회지
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    • 제10권2호
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    • pp.34-43
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    • 2018
  • Silicon has become of increasing importance as the basic element of many high-technology products. Its synthesis is very difficult requiring high temperature solid-state reactions (> $1000^{\circ}C$) or lower temperature methods ($100-200^{\circ}C$) involving hydrothermal and solvothermal reactions under extreme pH conditions. In nature, on the other hand, a wide range of living organisms have collectively evolved the means of biosilicification at the astounding rate of gigatons/year. This is impressive because biosilicification in these organisms occurs under mild physiological conditions. Marine sponges possess the ability to sequester soluble silicon sources from their environments and assemble them into intricate 3D architecture. The advent of molecular biology has recently made it possible to glean molecular information about biosilicification from these systems and it turned out that enzyme silicatein is the core of biosilicification. In this review, biosilicification regulated by silicatein and its mechanism are described. Also, production of silicatein through recombinant technology and several applications of recombinant silicatein are described including immobilization of silicatein, formation of Au or Ag nanoparticles on nanowires, nanolithography approaches, core-shell materials, encapsulation, bone replacement materials, and microstructured optical fibers.

버네사이트 합성 시 합성 방법 및 양이온 조건에 따른 생성 광물 및 열수처리 후 상전이 특성 (Mineral Products and Characteristics of Phase Transformation after Hydrothermal Treatment according to the Synthetic Method and Cation Combination during Birnessite Synthesis)

  • 민소영;김영규
    • 자원환경지질
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    • 제52권6호
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    • pp.509-517
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    • 2019
  • 망간단괴를 주로 이루고 있는 망간산화물 버네사이트(7Å manganate, δ-MnO2)는 지표의 주요한 망간 광물로서 다양한 합성법이 연구되어 있으며 또한 토도로카이트 합성의 전구물질이기도 하다. 본 연구에서는 기존에 연구된 합성방법들 가운데 산화-환원반응을 합성기작으로 하는 Feng et al.(2004)와 Luo et al.(1998)의 방법, 환원반응을 합성기작으로 하는 Ma et al.(1999)의 방법 총 3 가지 방법을 참고하여 버네사이트 합성 조건 중 합성에 사용되는 염기(OH-)와 과망간산(MnO4-) 시약의 양이온 종류에 따른 합성 결과물의 특성을 연구하였다. 합성 시약의 양이온을 Na+와 K+ 두 이온으로 조합하여 총 12 가지 버네사이트를 합성하였다. 합성한 버네사이트의 구성 광물종은 XRD를 통해 동정하고 ICP를 통해 광물내의 두 이온 조성비를 측정하였다. 버네사이트를 전구물질로 한 부저라이트(buserite)를 열수처리한 생성물에 대한 XRD 분석 후 토도로카이트로의 상변이 유무 및 양상을 비교하였다. 그 결과 합성 방법마다 부산물 및 상전이 특성이 다른 경향성으로 나타났으며, 산화-환원반응기작 합성 방법에서 두 방법 모두 허스마나이트(hausmannite, γ-Mn3O4)와 페이크네타이트(feitknechtite, β-MnOOH)가 부산물로 생성되었다. Feng et al.(2004)의 방법에서는 망가나이트(manganite, γ-MnOOH) 상이 Na+가 지배적으로 존재하는 조건에서만 나타났다. 산화-환원반응 기작으로 합성한 두 가지 버네사이트는 공통적으로 NaOH, KMnO4를 사용하여 합성한 시료에서 토도로카이트(todorokite, 10Å manganate, OMS-1)로의 상전이가 나타났다. Ma et al.(1999)의 방법에서는 단일 상의 버네사이트가 합성되었고, 양이온을 Na+으로만 합성한 시료에서만 상전이를 확인하였다.

산화아연 나노핵의 조작을 통한 산화아연 나노로드의 제어 (Artificial Control of ZnO Nanorods via Manipulation of ZnO Nanoparticle Seeds)

  • 신경식;이삼동;김상우
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2008년도 추계학술대회 논문집 Vol.21
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    • pp.399-399
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    • 2008
  • Synthesis and characterization of ZnO structure such as nanowires, nanorods, nanotube, nanowall, etc. have been studied to multifunctional application such as optical, nanoscale electronic and chemical devices because it has a room-temperature wide band gap of 3.37eV, large exiton binding energy(60meV) and various properties. Various synthesis methods including chemical vapor deposition (CVD), physical vapor deposition, electrochemical deposition, micro-emulsion, and hydrothermal approach have been reported to fabricate various kinds of ZnO nanostructures. But some of these synthesis methods are expensive and difficult of mass production. Wet chemical method has several advantage such as simple process, mass production, low temperature process, and low cost. In the present work, ZnO nanorods are deposited on ITO/glass substrate by simple wet chemical method. The process is perfomed by two steps. One-step is deposition of ZnO seeds and two-step is growth of ZnO nanorods on substrates. In order to form ZnO seeds on substrates, mixture solution of Zn acetate and Methanol was prepared.(one-step) Seed layers were deposited for control of morpholgy of ZnO seed layers by spin coating process because ZnO seeds is deposited uniformly by centrifugal force of spin coating. The seed-deposited samples were pre-annealed for 30min at $180^{\circ}C$ to enhance adhesion and crystallinnity of ZnO seed layer on substrate. Vertically well-aligned ZnO nanorods were grown by the "dipping-and-holding" process of the substrates into the mixture solution consisting of the mixture solution of DI water, Zinc nitrate and hexamethylenetetramine for 4 hours at $90^{\circ}C$.(two-step) It was found that density and morphology of ZnO nanorods were controlled by manipulation of ZnO seeds through rpm of spin coating. The morphology, crystallinity, optical properties of the grown ZnO nanostructures were carried out by field-emission scanning electron microscopy, high-resolution electron microscopy, photoluminescence, respectively. We are convinced that this method is complementing problems of main techniques of existing reports.

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다양한 합성 방법으로 제조된 BiFe0.65MoP0.1 산화물 촉매 상에서 n-부텐의 산화탈수소화 반응 (Oxidative Dehydrogenation of n-Butenes over BiFe0.65MoP0.1 Oxide Catalysts Prepared with Various Synthesis Method)

  • 박정현;신채호
    • Korean Chemical Engineering Research
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    • 제53권3호
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    • pp.391-396
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    • 2015
  • n-부텐의 산화탈수소화에서 제조방법이 촉매의 반응활성에 미치는 영향을 조사하기 위하여 $BiFe_{0.65}MoP_{0.1}$ 산화물 촉매를 모델 촉매로 선정하여 공침법, 시트르산법, 수열합성법, 주형법 등의 방법으로 촉매를 제조하였다. 제조한 촉매의 물리 화학적 특성을 알아보고 반응 활성과 연관시키기 위하여 X-선 회절분석(XRD), 질소 흡착 탈착분석($N_2$ sorption), 암모니아/1-부텐-승온탈착분석($NH_3/1$-butene-TPD) 등의 특성분석을 수행하였다. 공침법으로 제조한 촉매의 활성이 가장 높게 관찰되었으며, 14시간 동안의 산화탈수소화 반응 기준으로 n-부텐의 전환율은 79.5%, 1,3-부타디엔의 선택도는 85.1%, 1,3-부타디엔 수율은 67.7%의 수치를 보였다. 암모니아 승온탈착 실험으로부터 촉매의 반응 활성은 촉매의 산특성과 밀접하게 관련이 있으며, 공침법으로 제조한 산화물 촉매가 다른 합성방법으로 제조한 촉매와 비교하여 가장 큰 산량을 갖는 것으로 관찰되었다. 또한, 1-부텐의 승온탈착 분석결과, 촉매의 활성은 흡착된 1-부텐과 촉매의 표면반응에 기인한 중간체의 흡 탈착 특성, 즉 약하게 흡착된 중간체(< $200^{\circ}C$)의 상대적인 양과 강하게 흡착된 중간체의 탈착 온도(> $200^{\circ}C$)와 밀접하게 관련이 있었다.