Porous graphene oxide (P-GO) was successfully synthesized by using a simple glucose mediated hydrothermal method form prepared graphene oxide (GO). Then the P-GO was characterized by X-ray Powder Diffraction (XRD), Fourier-Transform Infrared (FITR), Raman, Brunauer–Emmett–Teller (BET), Field Emission Scanning Electron Microscopy (FESEM) and Transmission Electron Microscopy (TEM) analysis to determine the crystallinity, surface functionality, surface defect, surface area and porous nature of the material. For the comparative properties studies with P-GO, the synthesised GO was also characterised using the aforementioned analytical techniques. The formation of macroporous 2D sheet-like structure of P-GO with pore size diameters of 0.2–0.5 μm was confirmed by FESEM and TEM images. The surface area of P-GO was found to be 1272 m2/ g which is much higher compare to GO (i.e., 172 m2/ g) because of porous structure. P-GO was used for the adsorptive removal of F− ions from water using batch adsorption method. The highest adsorption occurs in the pH range of 5–7 with maximum adsorption capacity of 1272 mg/g. The experimental data revealed that the adsorption process obeys Langmuir monolayer isotherm model. The kinetic analysis revealed that the adsorption procedure is extremely rapid and mainly fit to the Pseudo-second-order (PSO) model. The effect of co-existing ions on fluoride adsorption capacity by P-GO decreases in the following order: PO4 3− > CO3 2− > SO4 2− > HCO3 − > NO3 − > Cl−. The mechanism of adsorption of fluoride onto the P-GO surface includes electrostatic interactions and hydrogen bonding.
Tin-antimony sulfide nanocomposites were prepared via hydrothermal synthesis and a N2 reduction process for use as a negative electrode in a sodium ion battery. The electrochemical energy storage performance of the battery was analyzed according to the tin-antimony composition. The optimized sulfides exhibited superior charge/discharge capacity (770 mAh g-1 at a current density of 100 mA g-1) and stable lifespan characteristics (71.2 % after 200 cycles at a current density of 500 mA g-1). It exhibited a reversible characteristic, continuously participating in the charge-discharge process. The improved electrochemical energy storage performance and cycle stability was attributed to the small particle size, by controlling the composition of the tin-antimony sulfide. By optimizing the tin-antimony ratio during the synthesis process, it did not deviate from the solubility limit. Graphene oxide also acts to suppress volume expansion during reversible electrochemical reaction. Based on these results, tin-antimony sulfide is considered a promising anode material for a sodium ion battery used as a medium-to-large energy storage source.
Spherical Li3V2(PO4)3 (LVP) and carbon-coated LVP with a monoclinic phase for the cathode materials are synthesized by a hydrothermal method using N2H4 as the reducing agent and saccharose as the carbon source. The results show that single phase monoclinic LVP without impurity phases such as LiV(P2O7), Li(VO)(PO4) and Li3(PO4) can be obtained after calcination at 800 oC for 4 h. SEM and TEM images show that the particle sizes are 0.5~2 μm and the thickness of the amorphous carbon layer is approximately 3~4 nm. CV curves for the test cell are recorded in the potential ranges of 3.0~4.3 V and 3.0~4.8 V at a scan rate of 0.01 mV s–1 and at room temperature. At potentials between 3.0 and 4.8 V, the third Li+ ions from the carbon-coated LVP can be completely extracted, at voltages close to 4.51 V. The carbon-coated LVP exhibits an initial specific discharge capacity of 118 mAh g–1 in the voltage region of 3.0 to 4.3 V at a current rate of 0.2 C. The results indicate that the reducing agent and carbon source can affect the crystal structure and electrochemical properties of the cathode materials.
In the present work, we synthesize nano-sized ZnO, SnO2, and TiO2 powders by hydrothermal reaction using metal chlorides. We also examine the energy-storage characteristics of the resulting materials to evaluate the potential application of these powders to dye-sensitized solar cells. The control of processing parameters such as pressure, temperature, and the concentration of aqueous solution results in the formation of a variety of powder morphologies with different sizes. Nano-rod, nano-flower, and spherical powders are easily formed with the present method. Heat treatment after the hydrothermal reaction usually increases the size of the powder. At temperatures above 1000oC, a complete collapse of the shape occurs. With regard to the capacity of DSSC materials, the hydrothermally synthesized TiO2 results in the highest current density of 9.1 mA/cm² among the examined oxides. This is attributed to the fine particle size and morphology with large specific surface area.
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.
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.
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
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.
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.
Nanostructures of ZnO, such as nanowires, nanorods, nanorings, and nanobelts have been actively studied andapplied in electronic or optical devices owing to the increased surface to volume ratio and quantum confinement that theyprovide. ZnO seed layer (about 40nm thick) was deposited on Si(100) substrate by RF magnetron sputtering with power of60 W for 5 min. ZnO nanorods were grown on ZnO seed layer/Si(100) substrate at 95oC for 5 hr by hydrothermal methodwith concentrations of Zn(NO3)2·6H2O [ZNH] and (CH2)6N4 [HMT] precursors ranging from 0.02M to 0.1M. We observed themicrostructure, crystal structure, and photoluminescence of the nanorods. The ZnO nanorods grew with hexahedron shape tothe c-axis at (002), and increased their diameter and length with the increase of precursor concentration. In 0.06 M and 0.08M precursors, the mean aspect ratio values of ZnO nanorods were 6.8 and 6.5; also, ZnO nanorods had good crystal quality.Near band edge emission (NBE) and a deep level emission (DLE) were observed in all ZnO nanorod samples. The highestpeak of NBE and the lower DLE appeared in 0.06 M precursor; however, the highest peak of DLE and the lower peak ofNBE appeared in the 0.02 M precursor. It is possible to explain these phenomena as results of the better crystal quality andhomogeneous shape of the nanorods in the precursor solution of 0.06 M, and as resulting from the bed crystal quality and theformation of Zn vacancies in the nanorods due to the lack of Zn++ in the 0.02 M precursor.
본 연구에서는 올레산을 표면개질제로 사용하여 수열법을 통해 수산화 마그네슘을 합성하였다. 수산화 마그네슘은 알카리 조건에서 올레인산과의 반응을 통해 표면 개질된 마이크로 크기의 플레이크 형상을 갖는다. 수열합성에서 수산화 마그네슘 입자 생성의 조건은 pH, 온도 그리고 반응시간이 표면개질과 입자 형상의 주요 변수임을 확인하였다. 생성된 수산화 마그네슘 입자는 FE-SEM, XRD, FT-IR 그리고 TGA를 통해 확인하였다. 유기 용매 내에서의 분산성의 확인은 개질되지 않은 수산화 마그네슘과의 침전 테스트 비교를 통해 확인하였다.
Ag spot-coated Cu nanopowders were synthesized by a hydrothermal-attachment method (HA) using oleic acid capped Ag hydrosol. Cu nano powders were synthesized by pulsed wire exploding method using 0.4 mm in diameter of Cu wire (purity 99.9%). Synthesized Cu nano powders are seen with comparatively spherical shape having range in 50 nm to 150 nm in diameter. The oleic acid capped Ag hydrosol was synthesized by the precipitation-redispersion method. Oleic acid capped Ag nano particles showed the narrow size distribution and their particle size were less than 20 nm in diameter. In the case of nano Ag-spot coated Cu powders, nanosized Ag particles were adhered in the copper surface by HAA method. The components of C, O and Ag were distributed on the surface of copper powder.
The pearlesent pigment has received attention in a diversity of fields like cosmetics, inks, paints and so on. Ferric Ferrocyanide, one of the nano sized pearlescent pigment, is a kind of surface modification pigment that covers a metal oxidized substance or a coloring agent with uniform thickness. Characteristics of pearlescent pigment are various interference color, intense gloss effect and a three-dimensional effect. We synthesised the pearlesent pigment that ferric ferrocyanide can be deposited on the titania/mica surface by hydrothermal synthesis method. The process parameters are concentration of precursor, controlling pH and reaction temperature. The optimun conditions is that amount of iron(III) chloride hexahydrate is 3.1 wt% and amount of potassim ferrocynide trihydrate is 3.6 wt% in the started pH 4.5 at 70℃. The coating rate and coating efficiency of ferric ferrocyanide was about 1.47 % and 96.7 %, respectively. The synthesised pearlesent pigment was characterized by SEM, XRD, FT-IR and EDS.
nanowires were synthesized by a hydrothermal reaction of metallic Y with aqueous solution of LiOH. The morphology and the size of the nanowires changed with varying the volume of the LiOH solution inside the autoclave. nanowires transformed to by a subsequent heat-treatment without morphological change. By a proper control of hydrothermal reaction parameter and heat-treatment, the yield of pure nanowires up to 97% was attained.
ZnO nanostructures were grown on an Au seed layer by a hydrothermal method. The Au seed layer was deposited by ion sputter on a Si (100) substrate, and then the ZnO nanostructures were grown with different precursor concentrations ranging from 0.01 M to 0.3M at 150˚C and different growth temperatures ranging from 100˚C to 250˚C with 0.3 M of precursor concentration. FE-SEM (field-emission scanning electron microscopy), XRD (X-ray diffraction), and PL (photoluminescence) were carried out to investigate the structural and optical properties of the ZnO nanostructures. The different morphologies are shown with different growth conditions by FE-SEM images. The density of the ZnO nanostructures changed significantly as the growth conditions changed. The density increased as the precursor concentration increased. The ZnO nanostructures are barely grown at 100˚C and the ZnO nanostructure grown at 150˚C has the highest density. The XRD pattern shows the ZnO (100), ZnO (002), ZnO (101) peaks, which indicated the ZnO structure has a wurtzite structure. The higher intensity and lower FWHM (full width at half maximum) of the ZnO peaks were observed at a growth temperature of 150˚C, which indicated higher crystal quality. A near band edge emission (NBE) and a deep level emission (DLE) were observed at the PL spectra and the intensity of the DLE increased as the density of the ZnO nanostructures increased.
우리는 마이카, boron nitride, bismuthoxychloride와 같은 판상 분체에 ZnO 나노입자를 코팅한 고 기능성 무기 분체를 합성하였다. 본 실험에서 우리는 수열침전법을 이용하여 합성 분체를 합성하였다. 출발물질은 ZnCl2를 사용하였고 침전제로는 hexamethylenetetramine(HMT)와 urea를 사용하였다. 본 실험의 반응변수로는 출발물질의 농도, 침전제 및 반응온도를 변화시켜 실험하였다. 합성물의 형태, 결정성 및 UV-차단능은FE-SEM, XRD, FT-IR, TGA-DTA, in vitro SPF 테스트를 활용해 분석하였다. 본 실험의 결과, 나토입자 크기를 갖는 ZnO는 동일한 최적의 합성조건하에서 다양한 판상 분체의 종류에 관계없이 균일하게 코팅되었다.
In this study, spherical pre-BaTiO3 particles are prepared by gelation and aging process in autoclave without catalysts. The (Ba-Ti) gel used as a starting material was prepared by aging mixtures of titanyl acylate with barium acetate aqueous solution([glacial acetic acid (AcOH)]/[titanium isopropoxide (TIP)] 4, [barium acetate]/[TIP] 1) at 45℃ for 48hrs. XRD and SEM results for the (Ba-Ti) gel sample at aging process showed that the gel was formed via aggregation of the fine particles. It seems to be the primary particles of bulk (Ba-Ti) gel amorphous, but the spatial arrangement of barium and titanium in the (Ba-Ti) gel is similar to that in crystalline BaTiO3 particles. From XRD and FT-IR. spectroscopy analysis it was found that the crystal structure of the prepared particles continuously transformed from amorphous to tetragonal as the calcination temperature increased, and crystallized spherical cubic and tetragonal BaTiO3 powder obtained at the very low calcination temperature between 500℃ and 900℃ after 1hrs of heat treatment respectively. According to BET analysis result, final particle have pore structure of ink bottle shape which is produced by aggregation of fine spherical particles with surface area of 280m2/g and average pore size of 130nm.