금속산화물 반도체 중 하나인 산화아연은 인체에 무해하고 친환경적이며, 우수한 화학적, 열 적 안정성의 특성을 지니며 3.37 eV의 넓은 밴드갭 에너지와 60 meV의 높은 엑시톤 바인딩 에너지로 인해 태양전지, 염료페기물의 분해, 가스센서 등 다양한 분야에 응용이 가능한 물질이다. 산화아연은 입 자 형상 및 결정성의 변화에 따라 광촉매 활성이 변하게 된다. 따라서, 다양한 실험변수와 첨가제를 사 용하여 입자를 합성하는 것이 매우 중요하다. 본 논문에서는 마이크로파 수열합성법을 사용하여 산화아연을 합성하였다. 전구체로는 질산아연을 사 용하였고, 수산화나트륨을 사용하여 용액의 pH를 11로 조정하였다. 첨가제로는 계면활성제인 에탄올아 민, 세틸트리메틸암모늄브로마이드, 소듐도데실설페이트, 솔비탄모노올레이트를 첨가하였다. 합성된 입자 는 별모양, 원추형, 씨드형태, 박막형태의 구형의 형상을 보였다. 합성된 산화아연의 물리・화학적 특성 은 XRD, SEM, TGA을 통하여 확인하였고, 광학적 특성은 UV-vis spectroscopy, PL spectroscopy, Raman spectroscopy으로 확인하였다.

본 연구에서는 고순도의 모데나이트(Mordenite) 입자를 합성하기 위하여 천연 제올라이트를 시드로 사용하여 시 드의 농도 및 수열합성 시간에 따른 천연 제올라이트 시드가 합성에 미치는 영향을 고찰하였다. 그 결과 시드가 입자의 형성 에 큰 영향을 끼치는 것을 확인할 수 있었고 시드를 3 g/100 g batch 주입하여 140°C에서 72시간 동안 수열합성을 진행하였 을 때 1-2 μm 사이즈의 고순도 모데나이트 입자를 합성할 수 있었다. 이를 통해 모데나이트 입자의 성장 기구를 규명할 수 있었으며, 모데나이트 입자 형성에 있어 시드는 첫째, 구형 모데나이트 전구체 형성 자리 공급의 역할과, 둘째 모데나이트 원 료 물질 소스 역할을 한다는 것을 알 수 있었다. 합성된 모데나이트 입자의 가스 흡착량 분석 결과 CO2 기체의 흡착량이 97.19 mg/g로 다른 가스들에 비해 비교적 높은 흡착성능을 보였으며, CO2/H2의 선택도가 가장 우수한 것으로 나타났다. 따라 서 이러한 결과들을 바탕으로 용도에 맞는 고순도 상의 모데나이트 입자를 합성할 수 있음을 확인하였고 보다 낮은 가격으로 우수한 분리성능을 갖는 분리막 소재개발에 활용할 수 있을 것이라 판단된다.

We report on an all-solution-processed hydrothermal method to control the morphology of ZnO nanostructures on Si substrates from three-dimensional hemispherical structures to two-dimensional thin film layers, by controlling the seed layer and the molar contents of surfactants during their primary growth. The size and the density of the seed layer, which is composed of ZnO nanodots, change with variation in the solute concentration. The ZnO nanodots act as heterogeneous nucleation sites for the main ZnO nanostructures. When the seed layer concentration is increased, the ZnO nanostructures change from a hemispherical shape to a thin film structure, formed by densely packed ZnO hemispheres. In addition, the morphology of the ZnO layer is systematically controlled by using trisodium citrate, which acts as a surfactant to enhance the lateral growth of ZnO crystals rather than a preferential one-dimensional growth along the c-direction. X-ray diffraction and energy dispersive X-ray spectroscopy results reveal that the ZnO structure is wurtzite and did not incorporate any impurities from the surfactants used in this study.

Flower-like nickel oxide (NiO) catalysts were coated on NiCrAl alloy foam using a hydrothermal method. The structural, morphological, and chemical bonding properties of the NiO catalysts coated on the NiCrAl alloy foam were investigated by field-emission scanning electron microscopy, scanning electron microscopy-energy dispersive spectroscopy, Xray diffraction, and X-ray photoelectron spectroscopy, respectively. To obtain flower-like morphology of NiO catalysts on the NiCrAl alloy foam, we prepared three different levels of pH of the hydrothermal solution: pH-7.0, pH-10.0, and pH-11.5. The NiO morphology of the pH-7.0 and pH-10.0 samples exhibited a large size plate owing to the slow reaction of the hydroxide (OH−) and nickel ions (Ni+) in lower pH than pH-11.5. Flower-like NiO catalysts (~4.7 μm-6.6 μm) were formed owing to the fast reaction of OH− and Ni2+ by increased OH− concentration at high pH. Thus, the flower-like morphology of NiO catalysts on NiCrAl alloy foam depends strongly on the pH of the hydrothermal solution.

본 연구에서는 고순도의 모데나이트 입자를 합성하기 위하여 천연 제올라이트를 시드로 사용하여 시드 농도 및 수열합성 시간에 따라 시드가 미치는 영향 을 고찰하였다. 시드를 3 g/100g batch 주입하여 140°C에서 72시간 동안 수열 합성 하였을 때 1-2 μm 사이즈의 고순도 모데나이트 입자를 안정적으로 합성할 수 있었다. 이를 통해 천연 제올라이트 시드는 모데나이트 입자의 성장에서 구형 모데나이트 전구체 형성 자리를 공급하고 모데나이트 원료 물질 소스 역 할을 한다는 것을 알 수 있었다. 이러한 결과들을 바탕으로 용도에 맞는 고순도 의 모데나이트 입자를 합성할 수 있음을 확인하였고 천연제올라이트를 사용함으로써 낮은 가격으로 우수한 성능을 갖는 소재개발에 활용할 수 있을 것이라 판단된다.

We report on the successful fabrication of ZnO nanorod (NR)/polystyrene (PS) nanosphere hybrid nanostructure by combining drop coating and hydrothermal methods. Especially, by adopting an atomic layer deposition method for seed layer formation, very uniform ZnO NR structure is grown on the complicated PS surfaces. By using zinc nitrate hexahydrate [Zn(NO3)2 ·6H2O] and hexamine [(CH2)6N4] as sources for Zn and O in hydrothermal process, hexagonal shaped single crystal ZnO NRs are synthesized without dissolution of PS in hydrothermal solution. X-ray diffraction results show that the ZnO NRs are grown along c-axis with single crystalline structure and there is no trace of impurities or unintentionally formed intermetallic compounds. Photoluminescence spectrum measured at room temperature for the ZnO NRs on flat Si and PS show typical two emission bands, which are corresponding to the band-edge and deep level emissions in ZnO crystal. Based on these structural and optical investigations, we confirm that the ZnO NRs can be grown well even on the complicated PS surface morphology to form the chestnut-shaped hybrid nanostructures for the energy generation and storage applications

In this work, uniform and nanosize(75nm) silicalite-1 crystals was hydrothermally synthesized by using 9TPAOH:0.16NaOH:25Si:495H2O solution at 80 ℃. They were applied as seed in the secondary growth process for preparing silicalite-1 membrane by template-free method. The highest ethanol/water separation factor of 119 with flux 0.58kg/m². Furthermore, these membranes (nano seed, template free silicalite-1 membrane) exhibit high permselectivity of He over SF6(123), and small gas permeation mechanism and Knudsen diffusion studies suggest that the membranes contain negligible intercrystalline or non-zeolite pores.

In the present work, a new synthesis method has been reported for preparing high-quality NaA zeolite membrane. The present method involves pressure-driven hydrothermal gel coating method(HGCM) on seeded α-alumina support surface having pores of 0.1 and 0.7μm diameter before the secondary growth process. The experimental data revealed that the high-pressure injection of hydrothermal gel solution on α-alumina support surface helped in the pore filling and thin layer coating of gel particles, which promoted the formation of uniform, defect free, and dense zeolite layer. Pervaporative dehydration experiments were conducted for 50 wt.% ethanol-water mixture at 343K. The NaA zeolite membrane, which was prepared by HGCM process on the 0.7μm support, showed that the high total flux was 4.7 kg m-2h-1 and separation factor was more than >1000.

Hydroxyapatite (HA), which is an important calcium phosphate mineral, has been applied in orthopedics, dentistry, and many other fields depending upon its morphology. HA can be synthesized with different morphologies through controlling the synthesis method and several parameters. Here, we synthesize various morphologies of HA using two simple methods: hydrothermal combustion and solution combustion. The phase purity of the synthesized HA is confirmed using X-ray diffractometry. It demonstrates that pure phased hydroxyapatite can be synthesized using both methods. The morphology of the synthesized powder is examined using scanning electron microscopy. The effects of pH and temperature on the final powder are also investigated. At 140 oC, using the hydrothermal method, nano-micro HA rods with a hexagonal crystal structure can be synthesized, whereas using solution combustion method at 600 oC, a dense cubic morphology can be synthesized, which exhibits monoclinic crystal structures.

Porous metallic glass compact (PMGC) are developed by electro-discharge sintering (EDS) process of gas atomized Zr41.2Ti13.8Cu12.5Ni10Be22.5 metallic glass powder under of 0.2 kJ generated by a 450 μF capacitor being charged to 0.94 kV. Functional iron-oxides are formed and growth on the surface of PMGCs via hydrothermal synthesis. It is carried out at 150oC for 48hr with distilled water of 100 mL containing Fe ions of 0.18 g/L. Consequently, two types of iron oxides with different morphology which are disc-shaped Fe2O3 and needle-shaped Fe3O4 are successfully formed on the surface of the PMGCs. This finding suggests that PMGC witih hydrothermal technique can be attractive for the practical technology as a new area of structural and functional materials. And they provide a promising road map for using the metallic glasses as a potential functional application.

석탄회를 NaOH로 용융시킨 후 수열 처리에 의하여 제올라이트 A를 합성하였다. NaOH/석탄회의 비, 용융 온도, NaAlO2의 첨가량, 수열 처리 온도 및 시간이 생성된 제올라이트의 종류와 결정도에 미치는 영향에 대하여 연구하였다. 결정도가 높은 제올라이트의 생성에 필요한 최적의 NaOH/석탄회의 중량비는 1.2, 최적의 용융 온도는 550℃이었다. 용융된 석탄회로부터 Si4+ 와 Al3+의 용출은 교반 시간의 영향을 받지 않았다. 생성된 제올라이트의 형태는 첨가한 NaAlO2의 영향을 받는 것으로 나타났다. 적은 양의 NaAlO2를 첨가하면 제올라이트 X가 생성되나 NaAlO2의 양이 증가하면 단일상의 제올라이트 A가 생성되었다. 수열처리 시간과 온도가 증가하면 제올라이트 A는 hydroxysodalite로 변화하였다. 승온 속도를 낮춰 반응 온도까지의 도달시간을 증가시키면 결정도가 좋은 제올라이트 A를 얻을 수 있었다.

In this work, uniform and nanosize(75nm) silicalite-1 crystals was hydrothermally synthesized by using 9TPAOH:0.16NaOH:25Si:495H2O solution at 80 ℃. They were applied as seed in the secondary growth process for preparing silicalite-1 membrane by template-free method. And silicalite-1 membrane, which was coated by nano-size seed, showed a high EtOH/H2O separation factor of 128. The high separation factor could be explained by the role of nanosize seed. The application of nanosize seed successfully retarded the formation of interfacial voids between silicalite-1 grains. Therefore, it could be concluded that template-free hydrothermal process can produce silicalite-1 membrane with well performance.

In the present work, a new synthesis method has been reported for preparing high-quality NaA zeolite membrane. The present method involves pressure-driven hydrothermal gel coating method(HGCM) on seeded α-alumina support surface having pores of 0.1 and 0.7μm diameter before the secondary growth process. The experimental data revealed that the high-pressure injection of hydrothermal gel solution on α-alumina support surface helped in the pore filling and thin layer coating of gel particles, which promoted the formation of uniform, defect free, and dense zeolite layer. Pervaporative dehydration experiments were conducted for 50 wt.% ethanol-water mixture at 343K. The NaA zeolite membrane, which was prepared by HGCM process on the 0.7μm support, showed that the high total flux was 4.7 kg m-2h-1 and separation factor was more than >1000.

Cubic mesocrystal CeO2 was synthesized via a hydrothermal method with glutamic acid (C5H9NO4) as a template. The XRD pattern of a calcined sample shows the face-centered cubic fluorite structure of ceria. Transmission electron microscopy (TEM) and the selected-area electron diffraction (SAED) pattern revealed that the submicron cubic mesocrystals were composed of many small crystals attached to each other with the same orientation. The UV-visible adsorption spectrum exhibited the red-shift phenomenon of mesocrystal CeO2 compared to commercial CeO2 particles; thus, the prepared materials show tremendous potential to degrade organic dyes under visible light illumination . With a concentration of a rhodamine B solution of 20 mg/L and a catalyst amount of 0.1 g/L, the reaction showed higher photocatalytic performance following irradiation with a xenon lamp (≥ 380 nm). The decoloring rate can exceed 100% after 300 min.

Recently, Korea’s municipal wastewater treatment plants generated amount of wastewater sludge per day. However, ocean dumping of sewage sludge has been prohibited since 2012 by the London dumping convention and protocol and thus removal or treatment of wastewater sludge from field sites is an important issue on the ground site. The hydrothermal carbonization is one of attractive thermo-chemical method to upgrade sewage sludge to produce solid fuel with benefit method from the use of no chemical catalytic. Hydrothermal carbonization improved that the upgrading fuel properties and increased materials and energy recovery ,which is conducted at temperatures ranging from 200 to 350°C with a reaction time of 30 min. Hydrothermal carbonization increased the heating value though the increase of the carbon and fixed carbon content of solid fuel due to dehydration and decarboxylation reaction. Therefore, after the hydrothermal carbonization, the H/C and O/C ratios decreased because of the chemical conversion. Energy retention efficiency suggest that the optimum temperature of hydrothermal carbonization to produce more energy-rich solid fuel is approximately 200°C.

We report the nitrogen monoxide (NO) gas sensing properties of p-type CuO-nanorod-based gas sensors. We synthesized the p-type CuO nanorods with breadth of about 30 nm and length of about 330 nm by a hydrothermal method using an as-deposited CuO seed layer prepared on a Si/SiO2 substrate by the sputtering method. We fabricated polycrystalline CuO nanorod arrays at 80˚C under the hydrothermal condition of 1:1 morality ratio between copper nitrate trihydrate [Cu(NO2)2·3H2O] and hexamethylenetetramine (C6H12N4). Structural characterizations revealed that we prepared the pure CuO nanorod array of a monoclinic crystalline structure without any obvious formation of secondary phase. It was found from the gas sensing measurements that the p-type CuO nanorod gas sensors exhibited a maximum sensitivity to NO gas in dry air at an operating temperature as low as 200˚C. We also found that these CuO nanorod gas sensors showed reversible and reliable electrical response to NO gas at a range of operating temperatures. These results would indicate some potential applications of the p-type semiconductor CuO nanorods as promising sensing materials for gas sensors, including various types of p-n junction gas sensors.

Photoelectrochemical cells have been used in photolysis of water to generate hydrogen as a clean energy source. A high efficiency electrode for photoelectrochemical cell systems was realized using a ZnO hierarchical nanostructure. A ZnO nanofiber mat structure was fabricated by electrospinning of Zn solution on the substrate, followed by oxidation; on this substrate, hydrothermal synthesis of ZnO nanorods on the ZnO nanofibers was carried out to form a ZnO hierarchical structure. The thickness of the nanofiber mat and the thermal annealing temperature were determined as the parameters for optimization. The morphology of the structures was examined by field-emission scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The performance of the ZnO nanofiber mat and the potential of the ZnO hierarchical structures as photoelectrochemical cell electrodes were evaluated by measurement of the photoelectron conversion efficiencies under UV light. The highest photoconversion efficiency observed was 63 % with a ZnO hierarchical structure annealed at 400˚C in air. The morphology and the crystalline quality of the electrode materials greatly influenced the electrode performance. Therefore, the combination of the two fabrication methods, electrospinning and hydrothermal synthesis, was successfully applied to fabricate a high performance photoelectrochemical cell electrode.

An effect of thermal annealing on activating phosphorus (P) atoms in ZnO nanorods (NR) grown using a hydrothermal process was investigated. NH4H2PO4 used as a dopant source reacted with Zn2+ ions and Zn3(PO4)2 sediment was produced in the solution. The fact that most of the input P elements are concentrated in the Zn3(PO4)2 sediment was confirmed using an energy dispersive spectrometer (EDS). After the hydrothermal process, ZnO NRs were synthesized and their PL peaks were exhibited at 405 and 500 nm because P atoms diffused to the ZnO crystal from the Zn3(PO4)2 particles. The solubility of the Zn3(PO4)2 initially formed sediment varied with the concentration of NH4OH. Before annealing, both the structural and the optical properties of the P-doped ZnO NR were changed by the variation of P doping concentration, which affected the ZnO lattice parameters. At low doping concentration of phosphorus in ZnO crystal, it was determined that a phosphorus atom substituted for a Zn site and interacted with two VZn, resulting in a PZn-2VZn complex, which is responsible for p-type conduction. After annealing, a shift of the PL peak was found to have occurred due to the unstable P doping state at high concentration of P, whereas at low concentration there was little shift of PL peak due to the stable P doping state.

Nano Pd spot-coated active carbon powders were synthesized by a hydrothermal-attachment method (HAA) using PVP capped Pd colloid in a high pressure bomb at , 450 psi, respectively. The PVP capped Pd colloid was synthesized by the precipitation-redispersion method. PVP capped Pd nano particles showed the narrow size distribution and their particle sizes were less than 8nm in diameter. In the case of nano Pd-spot coated active carbon powders, nano-sized Pd particles were adhered in the active carbon powder surface by HAA method. The component of Pd was homogeneously distributed on the active carbon surface.

Morphological control on hydroxyapatite crystals has attractive prospects in research to clarify the effects of crystal planes on biological performance. Hydrothermal processing is known as a typical type of processing for fabricating well-grown crystals with unique morphology. The purpose of the present study is to examine the feasibility of well-crystallized crystals with oriented structures through hydrothermal treatment of calcite. A single crystal of calcite was applied to hydrothermal treatment in a phosphate solution at 160˚C. Rod-shaped hydroxyapatite crystals with micrometer-size were formed on the 100 face of calcite after treatment, while nanometer-sized hydroxyapatite crystals were formed on the (111). The hydroxyapatite crystals formed on each plane were not morphologically changed with increasing treatment periods. An oriented structure of rod-shaped hydroxyapatite was constructed after hydrothermal treatment of 100 planes on the calcite single, while such orientation was not observed on the (111) plane after the treatment. The layer of hydroxyapatite formed on the 100 plane was thicker than that of the (111) plane. The 100 plane of calcite shows a higher reactivity than that of the (111) plane, which results in rapid crystal growth of hydroxyapatite. The difference in the morphology of the formed hydroxyapatite was governed by the reactivity of each crystal plane exposed to the surrounding solution.