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.
MoO3 metal oxide nanostructure was formed by hydrothermal synthesis, and a perovskite solar cell with an MoO3 hole transfer layer was fabricated and evaluated. The characteristics of the MoO3 thin film were analyzed according to the change of hydrothermal synthesis temperature in the range of 100 ℃ to 200 ℃ and mass ratio of AMT : nitric acid of 1 : 3 ~ 15 wt%. The influence on the photoelectric conversion efficiency of the solar cell was evaluated. Nanorod-shaped MoO3 thin films were formed in the temperature range of 150 ℃ to 200 ℃, and the chemical bonding and crystal structure of the thin films were analyzed. As the amount of nitric acid added increased, the thickness of the thin film decreased. As the thickness of the hole transfer layer decreased, the photoelectric conversion efficiency of the perovskite solar cell improved. The maximum photoelectric conversion efficiency of the perovskite solar cell having an MoO3 thin film was 4.69 % when the conditions of hydrothermal synthesis were 150 ℃ and mass ratio of AMT : nitric acid of 1 : 12 wt%.
Transition-metal oxide semiconductors have various band gaps. Therefore, many studies have been conducted in various application fields. Among these, methods for the adsorption of organic dyes and utilization of photocatalytic properties have been developed using various metal oxides. In this study, the adsorption and photocatalytic effects of WO3 nanomaterials prepared by hydrothermal synthesis are investigated, with citric acid added in the hydrothermal process as a structure-directing agent. The nanostructures of WO3 are studied using transmission electron microscopy and scanning electron microscopy images. The crystal structure is investigated using X-ray diffraction patterns, and the changes in the dye concentrations adsorbed on WO3 nanorods are measured with a UV-visible absorption spectrophotometer based on Beer-Lambert’s law. The methylene blue (MB) dye solution is subjected to acid or base conditions to monitor the change in the maximum adsorption amount in relation to the pH. The maximum adsorption capacity is observed at pH 3. In addition to the dye adsorption, UV irradiation is carried out to investigate the decomposition of the MB dye as a result of photocatalytic effects. Significant photocatalytic properties are observed and compared with the adsorption effects for dye removal.
Nano-sized Zinc selenide (ZnSe) powder was successfully synthesized using Zn and Se precursors in a hydrothermal process. Temperature for the synthesis was varied from 95 oC to 180 oC to evaluate its influence on the microstructural properties of the synthetic particles. ZnSe powder thus fabricated was characterized using various analytical tools such as SEM, XRD, TEM and UV-Vis methods. Two types of ZnSe particles, that is, the precipitated particle and the colloidal particles, were identified in the analysis. The precipitated particles were around 100 nm in average size, whereas the average size of the colloidal particles was around 20 nm. The precipitated particles made at 150 oC and 180 oC were found to be a single phase of ZnSe; however, an inhomogeneous phase was obtained at the lower synthesis temperature of 95 oC, suggesting that the temperature for the synthesis should be over 100 oC. The precipitated particles were inactive in the UV-Vis absorption investigation, whereas the colloidal particles showed that absorptions occurred at 380 nm in the UV-Vis spectrum.
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.
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.
1-D ZnO nanowires have been attractive for their peculiar properties and easy growth at relatively low temperature. The length, diameter, and density of ZnO nanowires were determined by the several synthetic parameters, such as PEI concentration, growth time, temperature, and zinc salt concentration. The ZnO nanowires were grown on the<001> oriented seed layer using the hydrothermal process with zinc nitrate and HMTA (hexamethylenetetramine) and their structure and optical properties were characterized. The morphology, length and diameter of the nanowires were strongly affected by the relative and/or absolute concentration of Zn2+ and OH-1 and the hydrothermal temperature. When the concentrations of the zinc nitrate HMTA were the same as 0.015 M, the length and diameter of the nanowires were 1.97μm and 0.07μm, respectively, and the aspect ratio was 28.1 with the preferred orientation along the<001> direction. XRD and TEM results showed a high crystallinity of the ZnO nanowires. Optical measurement revealed that ZnO nanowires emitted intensive stimulated UV at 376 nm without showing visible emission related to oxygen defects.
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.
The industrial manufacturing of YSZ products can be summarized as a three step process: a) hydrolysis of zirconyl chloride and mixing of other solutions, b) precipitation, and c) calcination. The addition of ammonia or OH- is essential in the precipitation process. However, a strong agglomeration was observed in the results of an ammonia or OH- addition. Thus, it is necessary to disperse the powders smoothly in order to improve the mechanical strength of YSZ. In this study, YSZ was synthesized using the urea stabilizer and hydrothermal method. YSZ powders were synthesized using a hydrothermal method with Teflon Vessels at 180˚C for 24 h. The mole ratio of urea to Zr was 0, 0.5, 1, and 2. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens (33 mm×8 mm×1±0.5 mm) for three-point bend tests were used in the mechanical properties evaluation. The crystalline of YSZ powders observed a tetragonal phase in the sample with a ratio of Zr:urea = 1:2 addition and a hydrothermal reaction time of 24 h. The average primary particle size of YSZ was measured to be 9 nm to 11 nm. The agglomerated particle size was measured from 15 nm to 30 nm. The three-point bending strength of the YSZ samples was 142.47 MPa, which is the highest value obtained for the Zr:urea = 1:2 ratio addition YSZ sample.
ZnO nanorods for gas sensors were prepared by a hydrothermal method. The ZnO gas sensors were fabricated on alumina substrates by a screen printing method. The gas-sensing properties of the ZnO nanorods were investigated for CH4 gas. The effects of growth time on the structural and morphological properties of the ZnO nanorods were investigated by X-ray diffraction and scanning electron microscope. The XRD patterns of the nanocrystallized ZnO nanorods showed a wurtzite structure with the (002) predominant orientation. The diameter and length of the ZnO nanorods increased in proportion to the growth time. The sensitivity of the ZnO sensors to 5 ppm CH4 gas was investigated for various growth times. The ZnO sensors exhibited good sensitivity and rapid response-recovery characteristics to CH4 gas, and both traits were dependent on the growth time. The highest sensitivity of the ZnO sensors to CH4 gas was observed with the growth time of 7 h. The response and recovery times were 13 s and 6 s, respectively.
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.
In this study, partially stabilized zirconia was synthesized using a chemical Y2O3 stabilizer and hydrothermal method. First, YCl3-6H2O and ZrCl2O-8H2O was dissolved in distilled water. Y-TZP (a Y2O3-doped toughened zirconia polycrystalline precursor) was also prepared by conventional co-precipitates in the presence of an excess amount of NH4OH solution under a fixed pH of 12. The Y-TZP precursors were filtered and repeatedly washed with distilled water to remove Cl- ions. ZrO2-Xmol%Y2O3 powder was synthesized by a hydrothermal method using Teflon Vessels at 180˚C for 6 h of optimized condition. The powder added with the Xmol%- Y2O3 (X = 0,1,3,5 mol%) stabilizer of the ZrO2 was synthesized. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens of 33mm×8mm×3 mm for three-point bend tests were used in the mechanical properties evaluation. A teragonal phase was observed in the samples, which contains more than 3 mol% Y2O3. The 3Y-ZrO2 agglomerated particle size was measured at 7.01μm. The agglomerated particle was clearly observed in the sample of 5 mol % Y2O3-ZrO2, and and the agglomerated particle size was measured at 16.4 um. However, a 20 nm particle was specifically observed by FE-SEM in the sample of 3 mol% Y2O3-ZrO2. The highest bending fracture strength was measured as 321.3 MPa in sample of 3 mol% Y2O3-ZrO2.
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.
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.
Submicron nickel powders were prepared from aqueous solution under hydrothermal condition. The experimental conditions including the types of protective agents, concentration of the solution and the pH were studied in detail. Starting concentration of nickel ion is a dominant factor affecting particle size. It was shown that the subsequent addition of Poly Vinyl Pyrrolidone(PVP) and Sodium Dodecyle Sulfate(SDS) can help to disperse the nickel powder. X-ray diffraction and SEM were employed to characterize the products.