• Applied Chemistry for Engineering
• /
• v.28 no.5
• /
• pp.593-596
• /
• 2017

Sodium titanate nanosheets were prepared by a hydrothermal synthesis method under basic conditions. Ruthenium was introduced on the surface of sodium titanate nanosheets through an UV irradiation in the aqueous $RuCl_3$ solution. The crystal phase and morphology of synthesized samples were analyzed by X-ray diffraction, transmission electron microscopy and energy dispersive spectroscopy. In addition, the content of Ru was evaluated by inductively coupled plasma. It was proposed that a monomeric form of ruthenium was incorporated on the surface of sodium titanate. Ruthenium incorporated sodium titanates were applied to alcohol oxidation using molecular oxygen as an oxidant. The sample with 7% ruthenium showed a catalytic activity with a turnover frequency value of $2.1h^{-1}$ in oxidizing benzyl alcohol to benzaldehyde without any other byproducts at $105^{\circ}C$ and 1 atmosphere.

• Resources Recycling
• /
• v.10 no.6
• /
• pp.29-34
• /
• 2001

Fly ash powders were refined and separated into fine and coarse size by multi-air classification, and each particle was used for synthesizing mullite and zeolite. Mullite was prepared by sintering the mixture of fine fly ash with mean size of 6.5 $\mu$m and $A1_2$$O_3$powder at above $1450^{\circ}C$. Zeolite was synthesized through hydrothermal reaction with coarse fly ash mean size of $56.3\mu$m in 3.5 M NaOH solution at $120^{\circ}C$. The whole range of particle size can be recycled through size classification into fine and coarse fractions, which are used for syntheses of inorganic materials.

• Journal of the Korean Applied Science and Technology
• /
• v.33 no.1
• /
• pp.23-29
• /
• 2016

Zinc oxide of hexagonal wurzite, is known as n-type semiconductor. It has a wide band gap energy of 3.37 eV and large exciton binding energy of 60 meV. It can be widely applied to gas sensors, laser diodes, dye-sensitized solar cells and degradation of dye waste. The use of microwave hydrothermal synthesis brings a rapid reaction rate, high yield, and energy saving. Amine additives control the different particle shapes because of the chelate effect and formation of hydroxide ion. In this study, zinc nitrate hexahydrate was used as zinc precursor. In addition, ethanolamine, ethylenediamine, diethylenetriamine, and hexamethylenetetramine are used as shape control agent. The pH value was controlled as 11 by NaOH. The shapes of zinc oxide are star-like, rod, flower-like, and circular cone. In order to analyze physical, chemical, and optical properties of ZnO with diverse amine additives, we used XRD, SEM, EDS, FT-IR, UV-Vis spectroscopy, and PL spectroscopy.

• Membrane Journal
• /
• v.29 no.3
• /
• pp.183-189
• /
• 2019

Amphiphilic PCZ-r-PEG random copolymer assisted solvothermal process is used to prepare mesoporous $TiO_2$ microspheres generated from nanoparticles by self-assembly method. Synthesized PCZ-r-PEG is characterized by Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), gel permeation chromatography (GPC) and transmission electron microscopy (TEM). The mesoporous $TiO_2$ are prepared by PCZ-r-PEG, glucose, water in tertrahydrofuran solution at $150^{\circ}C$ for 12 h and the $TiO_2$ microspheres are calcined at $550^{\circ}C$ for 30 min to further crystallize and organic residue are removed. Morphology and crystallization phase is characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) respectively. The mesoporous $TiO_2$ crystallized in pure anatase phase with diameter of $300{\pm}20nm$.

• Journal of Powder Materials
• /
• v.28 no.2
• /
• pp.127-133
• /
• 2021

One-dimensional (1D) piezoelectric nanostructures are attractive candidates for energy generation because of their excellent piezoelectric properties attributed to their high aspect ratios and large surface areas. Vertically grown BaTiO₃ nanotube (NT) arrays on conducting substrates are intensively studied because they can be easily synthesized with excellent uniformity and anisotropic orientation. In this study, we demonstrate the synthesis of 1D BaTiO₃ NT arrays on a conductive Ti substrate by electrochemical anodization and sequential hydrothermal reactions. Subsequently, we explore the effect of hydrothermal reaction conditions on the piezoelectric energy conversion efficiency of the BaTiO₃ NT arrays. Vertically aligned TiO₂ NT arrays, which act as the initial template, are converted into BaTiO₃ NT arrays using hydrothermal reaction with various concentrations of the Ba source and reaction times. To validate the electrical output performance of the BaTiO₃ NT arrays, we measure the electricity generated from each NT array packaged with a conductive metal foil and epoxy under mechanical pushings. The generated output voltage signals from the BaTiO₃ NT arrays increase with increasing concentration of the Ba source and reaction time. These results provide a new strategy for fabricating advanced 1D piezoelectric nanostructures by demonstrating the correlation between hydrothermal reaction conditions and piezoelectric output performance.

• Journal of Korean Society of Environmental Engineers
• /
• v.38 no.11
• /
• pp.603-610
• /
• 2016

This work studies the synthesis of birnessite (${\delta}-MnO_2$), a catalyst of oxidative-coupling reactions, from the powder of spent alkaline manganese batteries (SABP, <8 mesh) and evaluate its reactivity for 1-naphthol (1-NP) removals. Manganese oxides using commercial reagents ($MnSO_4$, $MnCl_2$) and the acid birnessite (A-Bir) by McKenzie method were also synthesized, and their crystallinity and reactivity for 1-NP were compared with one another. 96% Mn and 98% Zn were extracted from SABP by acid leaching at the condition of solid/liquid (S/L) ratio 1:10 in $1.0M\;H_2SO_4+10.5%\;H_2O_2$ at $60^{\circ}C$. From the acid leaching solution, 69% (at pH 8) and 94.3% (pH>13) of Mn were separated by hydroxide precipitation. Optimal OH/Mn mixing ratio (mol/mol) for the manganese oxide (MO) synthesis by alkaline (NaOH) hydrothermal techniques was 6.0. Under this condition, the best 1-NP removal efficiency was observed and XRD analysis confirmed that the MOs are corresponding to birnessite. Kinetic constants (k, at pH 6) for the 1-NP removals of the birnessites obtained from Mn recovered at pH 8 (${Mn^{2+}}_{(aq)}$) and pH>13 ($Mn(OH)_{2(s)}$) are 0.112 and $0.106min^{-1}$, respectively, which are similar to that from $MnSO_4$ reagent ($0.117min^{-1}$). The results indicated that the birnessite prepared from the SABP as a raw material could be used as an oxidative-coupling catalyst for removals of trace phenolic compounds in soil and water, and propose the recycle scheme of SAB for the birnessite synthesis.

• Journal of the Mineralogical Society of Korea
• /
• v.20 no.3
• /
• pp.147-153
• /
• 2007

Kaolinite [$Al_2Si_2O_5(OH)_4$] was successfully synthesized by a hydrothermal process from amorphous $Al(OH)_3$ and $SiO_2$ at $230^{\circ}C$ under the pressure of $30 kg/cm^2$. The experiments were performed varying temperatures ($180{\sim}280^{\circ}C$), pressure ($10{\sim}60kg/cm^2$), chemistry ($Al_2O_3/SiO_2 = 0.5{\sim}0.38$) and pH ($0.3{\sim}9.5$) of the solution. The autoclaving was carried out in a closed stainless steel vessel. Kaolinite appears from the starting composition of $Al_2O_3/SiO_2= 0.5$ with boehmite and was stable as a single phase with the composition of $Al_2O_3/SiO_2=0.45$. Boehmite was a stable phase below $200^{\circ}C$ for the 240 h period of autoclaving, but kaolinite appeared even in 20 h at $230^{\circ}C$. The single kaolinite phase of a good crystallinity was observed at pH ranging 2 to 6. That indicates that pH is one of the most critical parameters for the successful formation of kaolinite. The optimal molar ratio of $Al_2O_3$ to $SiO_2$ was determined to be 0.45. The XRD pattern of the synthesized kaolinite coincided with that of natural one and its morphology was the cluster type of the kaolinite crystals (diameter = ${\sim}3{\mu}m$), irrespective of starting material, composition and temperature.

• Journal of the Korean Chemical Society
• /
• v.44 no.1
• /
• pp.52-59
• /
• 2000

The reaction gel mixtures of molar composition (0.3${\sim}$2.1) $SiO_2:\;(0.10{\sim}0.50)\;CTABr:\;0.15{\sim}0.23)\;TMAOH:\;(20{\sim}100)\;H_2O$ we prepared and then aged at room temperature for a definite duration. The aged gel is reacted hydrothermally at $150^{\circ}C$ for 2 days. The pH of reaction gel during synthesis is strongly influenced by the concentration of TMAOH and silica source. The pH change affects the phase of product, which is monitored by X-ray diffractometer. With increasing the TMAOH ratio from 0.19 to 0.23, the gel becomes more basic, and the product involves more lamellar phase. At TMAOH ratio lower than 0.19, the hexagonal phase is lower with decrease of pH. The content of the lamellar phase increases at a lower $SiO_2$ concentration, and higher concentrations have a clear detrimental effect on the crystallinity ofMCM-41 due to an excess silica source. The best quality MCM-41 is synthesized from a reaction gel composition of $1.0\;SiO_2:\;0.27\;CTABr:\;0.19\;TMAOH:\;40\;H_2O$. The pH values of this gel, aged one for 24 hr, and reacted one at $150^{\circ}C$ for 2 days are 12.3, 11.5, and 10.5, respectively. Gel aging for 24 h is essential for preparing high quality MCM-41. Longer aging causes a decrease of hexagonal phase.

• Clean Technology
• /
• v.26 no.1
• /
• pp.7-12
• /
• 2020

Ti-SBA-15 catalysts doped with lanthanide ions (Ln/Ti-SBA-15) were successfully synthesized using conventional hydrothermal method. In addition, they were characterized by XRD, FT-IR, DRS, BET, and PL. The activity of these materials on the photocatalytic decomposition of methylene blue under ultraviolet light irradiation was also examined. Ti-SBA-15 catalysts doped with various lanthanide ions maintained their mesoporous structure. The pore size and pore volume of Ln/Ti-SBA-15 materials decreased but their surface area increased upon the doping of lanthanide ion. Ln/Ti-SBA-15 materials exhibited the type IV nitrogen isotherm with desorption hysteresis loop type H2, which was characteristic of mesoporous materials. The size of hysteresis increased in the doping of lanthanide ions on Ti-SBA-15 material. There was no absorption in the visible region (> 400 nm) regardless of the doping of lanthanide ions to TiO₂ particles, while the broad bands at 220 nm appeared at the Ln/Ti-SBA-15 samples, indicating the framework incorporation of titanium into SBA-15. 1 mol% Pr/ Ti-SBA-15 catalysts showed the highest photocatalytic activity on the decomposition of methylene blue but the Ti-SBA-15 catalysts doped with Eu, Er, and Nd ions showed lower activity compared to pure Ti-SBA-15 catalyst. The PL peaks appeared at about 410 nm at all catalysts while the excitonic PL signal was proportional to the photocatalytic activity for the decomposition of methylene blue.

• Transactions of the Korean hydrogen and new energy society
• /
• v.11 no.3
• /
• pp.119-125
• /
• 2000

To improve the photochemical energy conversion efficiency and the stability of CdS particulate film electrode which is used to produce hydrogen from the aqueous $H_2S$ solution photoelectrochemically, surface treatment of this film was carried out using $TiCl_4$ solution. CdS particles for preparation of the films were synthesized by precipitation reaction of $Cd({NO_3})_2{\cdot}9H_2O$ and $Na_2S{\cdot}4H_2O$. Then, the CdS sol was hydrothermally treated for 12hr in an autoclave with the variation of treatment temperature to control the crystalline phase of particles. CdS film electrode was thus prepared by annealing at $400^{\circ}C$ for 12hr of the wet-film cast at room temperature, and subsequently surface treated with $TiCl_4$ solution. The electrodes were characterized using XRD, SEM, and the photocurrent meter. The photocurrents of Cds film electrodes prepared with surface treatment were up to two times higher than the electrodes without surface treatment, indicating about $4.0mA/cm^2$. Hydrogen production rate in a continuous flow system using photoelectrochemical or photochemical cells prepared with surface treatment also increased in proportion to the increase of photocurrents.