Adsorption of vitamin E on mesoporous titania nanocrystals

Tri-block nonionic surfactant and titanium chloride were used as starting materials for the synthesis of mesoporous titania nanocrystallite powders. The main objective of the present study was to examine the synthesis of mesoporous titania nanocrystals and the adsorption of vitamin E on those nanocrystals using X-ray diffraction (XRD), transmission electron microscopy, and nitrogen adsorption and desorption isotherms. When the calcination temperature was increased to 300 °C, the reflection peaks in the XRD pattern indicated the presence of an anatase phase. The crystallinity of the nanocrystallites increased from 80% to 98.6% with increasing calcination temperature from 465 °C to 500 °C. The N₂ adsorption data and XRD data taken after vitamin E adsorption revealed that the vitamin E molecules were adsorbed in the mesopores of the titania nanocrystals.     

Mesoporous tin dioxide nanopowders based sensors to selectively detect ethanol vapor

In the paper, mesoporous SnO₂ nanopowders were synthesized via a simple and mild SnCl₄ hydrolysis process using cationic surfactant (cetyltrime thylammonium bromide, CTAB: CH₃(CH₂)₁₅N⁺(CH₃)₃Br^?) as structure directing agent and ammonia as an alkali source at room temperature, combined with a subsequent calcination process. The products were characterized by X-ray diffraction analysis (XRD), thermogravimetric analysis (TGA), transmission electron microscopy (TEM) and nitrogen adsorption–desorption experiment. A gas sensor was fabricated from the as-prepared mesoporous SnO₂ nanopowders and used to test the response to different concentrations of ethanol, methanol, hexane, NH₃, H₂ and CO at different operating temperatures. The results showed that the mesoporous SnO₂ sensor exhibited high sensitivity, good selectivity and quick response–recovery characteristics to ethanol, implying the potential application of the sensor for detecting ethanol.     

Preparation of nanocrystalline MgO by surfactant assisted precipitation method

Nanocrystalline magnesium oxide with high surface area was prepared by a simple precipitation method using pluronic P123 triblock copolymer (Poly (ethylene glycol)-block, Poly (propylene glycol)-block, Poly (ethylene glycol)) as surfactant and under refluxing conditions. The prepared samples were characterized by X-ray diffraction (XRD), N₂ adsorption (BET) and scanning and transmission electron microscopies (SEM and TEM). The obtained results revealed that the refluxing time and temperature and the molar ratio of surfactant to metal affect the structural properties of MgO, because of the changes in the rate and extent of P123 adsorption on the prepared samples. The results showed that the addition of surfactant is effective to prepare magnesium oxide with high surface area and affects the morphology of the prepared samples. With increasing the P123/MgO molar ratio to 0.05 the pore size distribution was shifted to larger size. The sample prepared with addition of surfactant showed a plate-like shape which was completely different with the morphology of the sample prepared without surfactant. The formation of nanoplate-like MgO was related to higher surface density of Mg ions on the (0 0 1) plane than that on the other planes of the Mg(OH)₂ crystal. The (0 0 1) plane would be blocked preferentially by the adsorbed P123 molecules during the growing process of Mg(OH)₂ nanoentities and the growth on the (0 0 1) plane would be markedly restricted, and the consequence is the generation of nanoplate-like MgO. In addition, increase in refluxing temperature and time increased the specific surface area of the prepared MgO samples.     

Synthesis of amorphous supermicroporous zirconium phosphate materials by nonionic surfactant templating

Supermicroporous zirconium phosphate materials possessing wormhole-like pores in the size range 1.3-1.8 nm were synthesized by using nonionic poly(ethylene oxide) surfactant (e.g., C₁₆H₃₃(EO)₁₀, C₁₈H₃₅(EO)₁₀) as a structure directing agent. The textural and structural properties were characterized by powder X-ray diffraction, N₂ adsorption analysis, differential thermal analysis, scanning and transmission electron microscopy, ³¹P MAS NMR and infrared spectroscopy. The synthesized materials are amorphous, exhibiting high surface areas, narrow pore size distributions, excellent thermal stabilities (over 800 °C) and acidic properties. The supermicropore size of the synthesized zirconium phosphate may be tunable by the variation of alkyl chain length of the surfactant.     

Synthesis and characterization of porous sphere-like ZnO with dendrite nanocrystals from layered inorganic-organic nanocomposite on titanium substrate

The porous sphere-like ZnO inorganic-organic nanocomposites have been prepared by self-assembly at the present of CTAB (cetyltrimethylammonium bromide, CH₃(CH₂)₁₅N⁺(CH₃)₃Br⁻) surfactant on the titanium substrate. After high temperature oxidation, all the organic were removed and the porous sphere-like ZnO dendrite nanocrystals were obtained. The resultant products have been characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The XRD pattern shows that the as-synthesized porous sphere-like is multilayered inorganic-organic nanocomposite, and the sample calcined at 500 °C for 2 h has a hexagonal wurtzite crystal structure. FE-SEM and TEM images demonstrate that porous sphere-like ZnO dendrite nanocrystals are formed. A possible formation mechanism is preliminary proposed for the formation of the novel nanostructure.     

High aspect ratio CdS nanowires synthesized in microemulsion system

CdS nanowires with typical length more than 8 μm and width of 30 nm on average have been successfully synthesized through Cd(NO₃)₂ reacting with CS₂ and ethylenediamine in microemulsion system of sodium dodecylbenzene sulfonate (SBDS). The microstructures of the as-synthesized CdS nanowires were characterized using XRD, transmission electron microscopy (TEM) and HRTEM. The possible formation mechanism was discussed. The morphologies of CdS sample strongly depend on the concentration of surfactant in solutions.     

Hydrothermal fabrication of various morphological α-Fe2O3 nanoparticles modified by surfactants

Two kinds of various morphological α-Fe₂O₃ nanoparticles modified by anionic surfactant (sodium dodecylsulfonate, SDS) and cationic surfactant (hexadecyipyridinium chloride, HPC), respectively, have been synthesized via hydrothermal method, using simple inorganic salt (NH₄)₃Fe(C₂O₄)₃ and alkali NaOH as starting precursors. Meanwhile, α-Fe₂O₃ nanoparticles without surfactant are also fabricated under the same conditions for comparison. The resultant products were characterized by means of Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron micrograph (TEM) combined with electron diffraction (ED) and magnetization measurements. It is interesting that the obtained α-Fe₂O₃ nanoparticles without surfactant are polyhedral with average particle size of 90 ± 35 nm; while the obtained α-Fe₂O₃ nanoparticles modified by SDS are ellipsoidal with mean particle size of major axis: ca. 420 nm; minor axis: ca. 205 nm and those modified by HPC are spherical with mean particle size of ca. 185 nm observed from TEM. In addition, magnetic hysteresis measurements reveal that the α-Fe₂O₃ nanoparticles modified by two surfactants show enhancement in coercivity (H_c) and the remanent magnetization (M_r) compared with those of the obtained α-Fe₂O₃ nanoparticles without surfactant at room temperature. The experimental results suggest that the surfactants not only significantly influence the size and shape of the particles, but also their magnetic properties.     

IF-WS2 nanoparticles size design and synthesis via chemical reduction

An innovative synthesis of inorganic fullerene-like disulfide tungsten (IF-WS₂) nanoparticles was developed using a chemical reduction reaction in a horizontal quartz reactor. In this process, first tungsten trisulfide (WS₃) was formed via a chemical reaction of tetra thiotungstate ammonium ((NH₄)₂WS₄), polyethylene glycol (PEG), and hydrochloric acid (HCl) at ambient temperature and pressure. Subsequently, WS₃ was reacted with hydrogen (H₂) at high temperature (1173-1373 K) in a quartz tube. The produced WS₂ nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), and transmission electron microscopy (TEM). The characterization results indicated that the high-purity (100%) IF-WS₂ nanoparticles were produced. Moreover, addition of surfactant (PEG) and higher operating temperature (1173-1373 K) decreased the particles agglomeration, and consequently led to the reduction of average diameter of WS₂ particles in the range of 50-78 nm. The developed method is simple, environmentally compatible, and cost-effective in contrast to the conventional techniques.     

Hydrothermal preparation, characterization and property research of flowerlike ZnO nanocrystals built up by nanoflakes

In the present paper, flowerlike ZnO nanocrystals were successfully synthesized via a simple hydrothermal route in the presence of sodium dodecyl sulfate (SDS), employing Zn(CH₃COO)₂ and KOH as the starting reactants. The phase and morphology of the product were characterized by means of powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and select area electron diffraction (SAED). The optical properties of the product were studied. Some factors influencing the morphology of the final product including reaction time, temperature and amounts of the surfactant were discussed. Researches showed that the flowerlike ZnO nanocrystals had a good photo-catalytic activity for degradation of safranine T under 254 nm UV light irradiation. The electrochemical research of the product showed that flowerlike ZnO nanocrystals could promote electron transfers between catechol and the Au electrode. A possible formation mechanism was also suggested based on the results of the experiments.     

Preparation and photoluminescence study of mesoporous indium hydroxide nanorods

Mesoporous indium hydroxide nanorods were successfully synthesized by a mild one-step one-pot method. The obtained samples were characterized by X-ray diffraction, transmission electron microscopy with selected area electron diffraction, N₂ adsorption, ultraviolet-visible absorption and photoluminescence, respectively. Transmission electron microscopy showed that there were some pores in the samples, which were mainly composed of rod-like shapes with length of 300 nm and diameter of 90 nm. N₂ adsorption/desorption measurements confirmed that the prepared powder was mesoporous with average pore diameter of 3.1 nm. The ultraviolet-visible absorption spectroscopy analysis indicated that the band gap energy of the samples was 5.15 eV. Photoluminescence spectrum showed that there were two strong emissions under ultraviolet light irradiation. The growth mechanism of indium hydroxide nanorods and the role of cetyltrimethyl ammonium bromide were also discussed.     

Morphology-controlled synthesis of ZnS nanostructures via single-source approaches

ZnS nanoparticles of various morphologies, including hollow or solid spherical, and polyhedral shape, were synthesized from single-source precursor Zn(S₂COC₂H₅)₂ without using a surfactant or template. The as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy. The results indicate that ZnS hollow and solid spheres assembled by nanoparticles can be easily generated by the solution phase thermalysis of Zn(S₂COC₂H₅)₂ at 80 °C using N, N-dimethylformamide (DMF) and ethylene glycol (EG) or water as solvents, respectively, whereas solvothermal process of the same precursor led to ZnS nanoparticles of polyhedral shape with an average size of 120 nm. The optical properties of these ZnS nanostructures were investigated by room-temperature luminescence and UV-vis diffuse reflectance spectra.     

Synthesis of hierarchical Ni11(HPO3)8(OH)6 superstructures based on nanorods through a soft hydrothermal route

In this paper, we reported the successful synthesis of hierarchical Ni₁₁(HPO₃)₈(OH)₆ superstructures based on nanorods via a facile hydrothermal route, employing NiCl₂·6H₂O and NaH₂PO₂·H₂O as the reactants in the presences of polyvinylpyrrolidone (PVP) and CH₃COONa·3H₂O. The reaction was carried out at 170 °C for 10 h. HPO₃²⁻ ions were provided via the dismutation reaction of H₂PO₂⁻ ions in a weak basic solution. The as-obtained products were characterized by X-ray powder diffraction (XRD), energy dispersive spectrometry (EDS), field emission scanning electron microscopy (SEM), selected area electron diffraction (SAED) and high resolution transmission electron microscopy (HRTEM). Some factors influencing the morphology of the hierarchical Ni₁₁(HPO₃)₈(OH)₆ nanorods, such as the reaction temperature, time, the amounts of PVP and CH₃COONa, and the initial concentration of Ni²⁺ ions, were systematically investigated. A possible growth mechanism was proposed based on experimental results.     

Preparation and characterization of CuO nanorods by thermal decomposition of CuC2O4 precursor

Synthesis of copper oxide (CuO) nanorods was achieved by thermal decomposition of the precursor of CuC₂O₄ obtained via chemical reaction between Cu(CH₃COO)₂·H₂O and H₂C₂O₄·2H₂O in the presence of surfactant nonyl phenyl ether (9)/(5) (NP-9/5) and NaCl flux. Transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), selected-area electron diffraction (SAED) and high-resolution TEM (HRTEM) were used to characterize the structure features and chemical compositions of the as-made nanorods. The results showed that the as-prepared nanorods is composed of CuO with diameter of 30-100 nm, and lengths ranging from 1 to 3 μm. The mechanism of formation of CuO nanorods was also discussed.     

A new and effective chemical reduction method for preparation of nanosized silver powder and colloid dispersion

Nanosized uniform silver powders and colloidal dispersions of silver were prepared from AgNO₃ by a chemical reduction method involving the intermediate preparation of Ag₂O colloidal dispersion in the presence of sodium dodecyle sulfate CH₃(CH₂)₁₁OSO₃Na as a surfactant. Several reducing agents such as hydrazine hydrate (N₂H₄·H₂O), formaldehyde (HCOH) and glucose (C₆H₁₀O₅) have been found to be preferable in this study from a practical point of view. The silver powder with the 60-120 nm particle size and colloidal dispersion with the particles size 10-20 nm and 0.5-2.0 wt.% concentration were successfully synthesized.     

Shape evolution of Cu2S nanostructures in Triton X-100/cyclohexane/water reverse micelles

The shape evolution of Cu₂S nanostructures, which were produced in Triton X-100/cyclohexane/water reverse micelles, was investigated by the transmission electron microscopy technique as a function of aging time, and the effect of the molar ratio of water to surfactant on the size and shape of Cu₂S nanostructures was also discussed. The results suggest that at the initial stage the nucleation process was dominant and the shape of Cu₂S nanostructures was preferably confined by the reverse micelle droplets and took spherical forms. With the extension of the aging time, the growth gradually governed the process and the shape of Cu₂S nanostructures evolved first to nanorods, and then to nanowires gradually. The formation of one-dimensional Cu₂S nanostructures is attributed to a directed aggregation growth process mediated by reverse micelle droplets, which was confirmed by high-resolution transmission electron microscopy. Furthermore, the size and shape of Cu₂S nanostructures can be controlled by changing the molar ratio of water to surfactant.     

Electron beam induced structural evolution in Fe3O4\SiO2 particles: A new route to obtain movable core structures

SiO₂ hollow spheres with movable Fe₃O₄ core were obtained by exposing the pre-synthesized Fe₃O₄\SiO₂ particles (with an adsorption interlayer of ethylene glycol) under the irradiation of electron beam inside transmission electron micrograph (TEM). In the formation process, the evaporation of adsorbed ethylene glycol and the evolution of amorphous SiO₂ layer played important roles, and that should be attributed to the high temperature and trapped charges induced by the irradiation of electron beam. This work provided a new route to obtain particles with movable core structure and extended the applications of electron beam.     

The effect of solution chemistry on the preparation of MgAl2O4 by hydrothermal-assisted sol-gel processing

Preparation of magnesium aluminate spinel powder by hydrothermal-assisted sol-gel processing from MgAl₂(OCH₂CH₂OR)₈, RCH₃ (1), CH₂CH₂OCH₃ (2), MgAl₂[OCH(CH₃)₂]₈ (3) and MgAl₂(O-^sBu)₈ (4) in toluene and parent alcohol has been investigated. Coordination status of aluminum atom in precursors was determined by ²⁷Al NMR and correlation between coordination number of aluminum and development of spinel phase in hydrothermal-assisted sol-gel processing has been studied. The gels obtained from hydrothermal-assisted hydrolysis of magnesium-aluminum alkoxides that contain six-coordinated aluminum atoms in solution (1 and 2) after calcination at 700 °C resulted in the formation of pure spinel phase, whereas in similar hydrolysis and calcination processes of precursors that contain four-coordinated aluminum (3 and 4) spinel phase forms along with some Al₂O₃ and MgO. Selected powders obtained from hydrothermal-assisted sol-gel processing were characterized by thermal analysis (TGA/DSC), X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). Results indicate that the coordination status of aluminum in the precursor is very crucial for the formation of pure phase spinel. The morphology of prepared spinels was studied by SEM and the results showed that the solvent in hydrothermal-assisted sol-gel processing has a marked effect on the morphology of the resulting MgAl₂O₄. In hydrothermal-assisted sol-gel processing of aluminum-magnesium alkoxides in hydrophobic solvent, spherical particles are formed, while in the parent alcohol, non-spherical powders are formed.     

Adsorption of mercury cation on chemically modified clay

A montmorillonite clay (M) sample from the Amazon region, Brazil, was intercalated with pyridine (Py), dimethyl sulfoxide (DS) and 3-aminopropyltriethoxysilane (APS). The chemically modified montmorillonite (M_P/APS) sample showed modification of its physical-chemical properties including: specific area 41.39 m² g⁻¹ (M) to 198.45 m² g⁻¹ (M_P/APS). Solid-state ²⁹Si CPMAS/NMR of the silylated montmorillonite samples showed Q² and Q³ signals as well as T² and T³ signals. The appearance of T² and T³ signals can be attributed to the grafting of APS to the interlayer surface silanol groups. The natural and modified clays were used for mercury cation adsorption from aqueous solutions at room temperature and pH 3.0. The energetic effects (Δ_intH°, Δ_intG° and Δ_intS°) caused by mercury cation adsorption were determined through calorimetric titrations.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.     

Hydrothermal preparation of fractal dendrites: Cerium carbonate hydroxide and cerium oxide

The surfactant-assisted hydrothermal route was used to prepare fractal dendrite cerium carbonate hydroxide (CeOHCO₃) microstructures. After annealing at 600 °C for 4 h, the products were transformed to CeO₂. The crystal structures of the two compounds were determined by X-ray diffraction (XRD). The morphologies and microstructures were characterized by field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM). Room temperature photoluminescence (PL) showed that a strong ultraviolet emission at 336 nm was observed for CeOHCO₃, and that centered at 415 nm for CeO₂ microstructures. Both of these emission peaks are different from those reported for CeOHCO₃ and CeO₂ with other shapes. In addition, the possible growth mechanism of dendrite CeOHCO₃ microstructures and the role of surfactant polyvinyl pyrrolidone (PVP) were also investigated in this paper.