Synthesis of NaP zeolite at room temperature and short crystallization time by sonochemical method

NaP zeolite nano crystals were synthesized by sonochemical method at room temperature with crystallization time of 3 h. For comparison, to insure the effect of sonochemical method, the hydrothermal method at conventional synthesis condition, with same initial sol composition was studied. NaP zeolites are directly formed by ultrasonic treatment without the application of autogenous pressure and also hydrothermal treatment. The effect of ultrasonic energy and irradiation time showed that with increasing sonication energy, the crystallinity of the powders decreased but phase purity remain unchanged. The synthesized powders were characterized by XRD, IR, DTA TGA, FESEM, and TEM analysis. FESEM images revealed that 50 nm zeolite crystals were formed at room temperature by using sonochemical method. However, agglomerated particles having cactus/cabbage like structure was obtained by sonochemical method followed by hydrothermal treatment. In sonochemical process, formation of cavitation and the collapsing of bubbles produced huge energy which is sufficient for crystallization of zeolite compared to that supplied by hydrothermal process for conventional synthesis. With increasing irradiation energy and time, the crystallinity of the synthesized zeolite samples increased slightly.     

Mechanistic investigation of the sonochemical synthesis of zinc ferrite

In this investigation, an attempt has been made to establish the physical mechanism of sonochemical synthesis of zinc ferrite with concurrent analysis of experimental results and simulations of cavitation bubble dynamics. Experiments have been conducted with mechanical stirring as well as under ultrasound irradiation with variation of pH and the static pressure of the reaction medium. Results of this study reveal that physical effects produced by transient cavitation bubbles play a crucial role in the chemical synthesis. Generation of high amplitude shock waves by transient cavitation bubbles manifest their effect through in situ micro-calcination of metal oxide particles (which are generated through thermal hydrolysis of metal acetates) due to energetic collisions between them. Micro-calcination of oxide particles can also occur in the thin liquid shell surrounding bubble interface, which gets heated up during transient collapse of bubbles. The sonochemical effect of production of OH radicals and H₂O₂, in itself, is not able to yield ferrite. Moreover, as the in situ micro-calcination involves very small number of particles or even individual particles (as in intra-particle collisions), the agglomeration between resulting ferrite particles is negligible (as compared to external calcination in convention route), leading to ferrite particles of smaller size (6 nm).     

Ultrasound-assisted synthesis of magnesium hydroxide nanoparticles from magnesium

Acoustic cavitation in water provides special kinetic and thermodynamic conditions for chemical synthesis and nanostructuring of solids. Using cavitation phenomenon, we obtained magnesium hydroxide from pure magnesium. This approach allows magnesium hydroxide to be synthesized without the requirement of any additives and non-aqueous solvents. Variation of sonochemical parameters enabled a total transformation of the metal to nanosized brucite with distinct morphology. Special attention is given to the obtaining of platelet-shaped, nanometric and de-agglomerated powders. The products of the synthesis were characterized by transmission electron microscopy (TEM), electron diffraction (ED), scanning electron microscopy (SEM) and X-ray diffraction (XRD).     

Facile sonochemical synthesis of nanosized InP and GaP

A novel sonochemical method for the preparation of MP (M = Ga, In) nanocrystalline materials has been developed. The procedure consists of the in situ synthesis of sodium phosphide and its subsequent reaction with the appropriate metal chloride using ultrasound. The products were characterized by X-ray powder diffraction, electron microscopy, and energy dispersive X-ray microanalysis (EDX). The choice of solvent and the use of high-power ultrasound are both important in the formation of the products.     

Sonochemical synthesis of silver nanorods by reduction of sliver nitrate in aqueous solution

The sonochemical synthesis of sliver nanorods has been achieved by ultrasonic irradiation of the aqueous solution of sliver nitrate, methenamine (HMTA) and poly (vinyl pyrrolidone) (PVP) for 60 min. The silver nanorods obtained have lengths of 4–7 μm and mean diameters of about 100 nm. The structures of the samples were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), selected area electron diffraction (SAED) and X-ray powder diffraction (XRD), and the chemical composition of the sample was examined by energy-dispersive X-ray spectrum (EDS). The effects of the irradiation time, the concentration of PVP and the reaction temperature on the morphology of silver nanorods were discussed, and the mechanism of the silver nanorods formation was tentatively inferred.     

Ultrasonic-assisted environmentally-friendly synergetic synthesis of nitroaromatic compounds in core/shell nanoreactor: A green protocol

An efficient sonochemical protocol for the nitration of aromatic compounds was described in the presence of a catalytic amount of sulfuric acid-functionalized silica-based core/shell magnetic nanocomposite at room temperature in an eco-friendly and recyclable media, deep eutectic solvent (DES), based on choline chloride and urea. The particle size, morphology and elemental analysis of the core/shell nanocatalyst were carried out by TEM, SEM, EDX and XRD analyses. The nanocatalyst and DES were easily recovered from the reaction mixture quantitatively and reused several times.     

Intensification of ultrasound-assisted process for the preparation of spindle-shape sodium zinc molybdate nanoparticles

In the present work, sodium zinc molybdate (SZM) nanoparticles were prepared using conventional and an innovative ultrasound assisted co-precipitation of sodium molybdate, zinc oxide and HNO₃ at different temperatures. Prepared product was characterized by XRD, TEM, FT-IR, particle size distribution (PSD), TGA and DTA techniques. TEM analysis shows the spindle-shaped morphology of the formed SZM nanoparticles. The average particle size of SZM nanoparticles is found to be lower in case of sonochemical method (78.3 nm) compared to conventional method (340.2 nm) which is attributed to faster solute transfer rate due to ultrasonic irradiation leading to rapid nucleation and restricted growth of SZM nanoparticles. Further, the kinetics of synthesis of SZM nanoparticles are studied using the sonochemical method at different operating temperature and conventional method at 80 °C. It is shown that the rate of reaction is significantly faster at 40 °C compared to other temperatures and also conventional method. This can be attributed to intense cavity collapse at lower temperature (low vapour pressure) compared to higher temperature (high vapour pressure) of the reaction mixture.     

Fabrication and characterization of silver/titanium dioxide composite nanoparticles in ethylene glycol with alkaline solution through sonochemical process

This paper aims to study fabrication and characterization of silver/titanium oxide composite nanoparticle through sonochemical process in the presence of ethylene glycol with alkaline solution. By using ultrasonic irradiation of a mixture of silver nitrate, the dispersed TiO₂ nanoparticle in ethylene glycol associated with aqueous solution of sodium oxide yields Ag/TiO₂ composite nanoparticle with shell/core-type geometry. The powder X-ray diffraction (XRD) of the Ag/TiO₂ composites showed additional diffraction peaks corresponding to the face-centered cubic (fcc) structure of silver crystallization phase, apart from the signals from the cores of TiO₂. Transmission electron microscopy (TEM) images of Ag/TiO₂ composites, which average particle size is roughly 80 nm, reveal that the titanium oxide coated by Ag nanoparticle with a grain size of about 2–5 nm. Additionally, the formation of silver nanoparticles on TiO₂ was monitored by ultraviolet visible light spectrophotometer (UV–Vis). As measured the optical absorption spectra of as-synthesized Ag nanoparticle varying with time, the mechanism of surface formatting silver shell on the cores of TiO₂ could be explored by autocatalytic reaction; the conversion of Ag particle from silver ion is 98% for the reaction time of 1000 s; and the activity energy of synthesizing Ag nanoparticles on TiO₂ is 40 kJ/mol at temperature ranging from 5 to 25 °C. Hopefully, this preliminary investigation could be used for mass production of composite nanoparticles assisted by ultrasonic chemistry in the future.     

Sonochemical preparation of SbSI gel

A novel sonochemical method for direct preparation of nanocrystalline antimony sulfoiodide (SbSI) has been established. The SbSI gel was synthesized using elemental Sb, S and I in the presence of ethanol under ultrasonic irradiation (35 kHz, 2 W/cm²) at 50 °C for 2 h. The products were characterized by using techniques such as powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and optical diffuse reflection spectroscopy (DRS). The SEM and HRTEM investigations exhibit that the as-prepared samples are made up of large quantity nanowires with diameters of about 10–50 nm and lengths reaching up to several micrometers and single-crystalline in nature.     

Sonochemical reaction of selected cyclic C6Hx hydrocarbons in organic solvents

The rates and products of the sonochemical reactions of benzene, 1,4-cyclohexadiene, 1,3-cyclohexadiene, cyclohexene, and cyclohexane in selected organic solvents have been investigated. The sonochemical reactions of these educts in the investigated organic solvents follow first-order kinetics. Generally, they are sonicated more rapidly in polar than in non-polar solvent; higher volatility of the solute results in faster sonolysis in the organic solvents. However, the sonication of cyclohexane in n-decane and the sonication of benzene in n-propanol are exceptional cases. Since cyclohexane exhibits a much higher lipophilicity and benzene a much higher hydrophilicity than other educts, it might be more difficult to transfer either educt from the bulk liquid into the cavitation bubbles. In tetrachloroethylene, the reactivity of the tested educts with in situ generated chlorine as well as chlorine-containing radical intermediates can accelerate the rate of sonochemical reactions under the employed conditions. In n-propanol and n-decane, the pyrolysis during the collapse of the cavitation bubbles is the only reaction pathway of sonolysis. In tetrachloroethylene, the pyrolysis during the collapse of the cavitation bubbles and the free radical reaction in the bulk liquid may occur simultaneously. Except for the products generated from sonolysis, products formed from chlorine transformations (substitution or addition reactions) are detected. Benzene is hardly decomposed in tetrachloroethylene. However, when FeCl3 is added into the reaction system, benzene is sonoconverted rapidly, and the product chlorobenzene was detected. In organic solvents, the sonoreaction rates and the sonoproducts are dependent on the physicochemical properties of the solvents used, as well as the volatility, the polarity and the reactivity of educts.     

Nanostructured TiO2 cavitation agents for dual-modal sonophotocatalysis with pulsed ultrasound

Current sonochemical methods rely on spatially uncontrolled cavitation for radical species generation to promote chemical reactions. To improve radical generation, sonosensitizers have been demonstrated to be activated by cavitation-based light emission (sonoluminescence). Unfortunately, this process remains relatively inefficient compared to direct photocatalysis, due to the physical separation between cavitation event and sonosensitizing agent. In this study, we have synthesized nanostructured titanium dioxide particles to couple the source for cavitation within a photocatalytic site to create a sonophotocatalyst. In doing so, we demonstrate that site-controlled cavitation from the nanoparticles using pulsed ultrasound at reduced acoustic powers resulted in the sonochemical degradation methylene blue at rates nearly three orders of magnitude faster than other titanium dioxide-based nanoparticles by conventional methods. Sonochemical degradation was directly proportional to the measured cavitation produced by these sonophotocatalysts. Our work suggests that simple nanostructuring of current sonosensitizers to enable on-site cavitation greatly enhances sonochemical reaction rates.     

Synthesis of CdS hollow/solid nanospheres and their chain-structures by membrane technique

CdS hollow/solid nanospheres and their chain-structures were successfully synthesized through supporting liquid membrane (SLM) system with bio-membrane. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), UV–Vis spectroscopy, and photoluminescence (PL) spectroscopy have been used for the characterization of the products. The average diameters of CdS solid/hollow spheres are about 10, 40 nm, respectively. The wall of the hollow spheres is about 5 nm. CdS products are all cubic face-centered structure with the cell constant a = 5.830 Å. We also explore the morphology, structure and possible synthesis mechanism. A possible template mechanism has been proposed for the production of the hollow CdS nanocrystals, that is, CdS nanoparticles grow along the non-soakage interface between CHCl3 and reactant solution. During this process, the organic functional groups were crucial to the control of crystal morphologies.     

Imaging the Hydrated Microbe‐Metal Interface Using Nanoscale Spectrum Imaging

PdAu nanocrystals are synthesised by Geobacter sulfurreducens, a dissimilatory metal‐reducing bacterium, and the resulting bimetallic nanocrystal‐decorated microbes are imaged using a range of advanced electron microscopy techniques. Specifically, the first example of elemental mapping of fully hydrated biological nanostructures using scanning transmission electron microscope (STEM) energy dispersive X‐ray (EDX) spectrum imaging within an environmental liquid‐cell is reported. These results are combined with cryo‐TEM and ex situ STEM imaging and EDX analysis with the aim of better understanding microbial synthesis of bimetallic nanoparticles. It is demonstrated that although Au and Pd are colocalized across the cells, the population of nanoparticles produced is bimodal, containing ultrasmall alloyed nanocrystals with diameters <3 nm and significantly larger core‐shell structures (>200 nm in diameter) which show higher Pd contents and exhibit a Pd enriched shell only a few nanometers thick. The application of high‐resolution imaging techniques described here offers the potential to visualize the microbe‐metal interface during the bioproduction of a range of functional materials by microbial “green” synthesis routes, and also key interfaces underpinning globally relevant environmental processes (e.g., metal cycling).     

Sonochemical synthesis of nanocrystalline mercury sulfide, selenide and telluride in aqueous solutions

Nanocrystalline mercury chalcogenides HgE (E = S, Se, Te) were synthesized in a single step by a convenient, simple sonochemical method. Mercury nitrate, Hg(NO₃)₂, dissolved in 0.1 M ethylenediamine tetraacetic acid (EDTA), was used as the source of mercury and elemental chalcogenes, dissolved in a NaOH solution, as the sources of chalcogenide. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDAX). The synthesis procedure is simple and uses less toxic reagents than the previously reported methods. The results showed that the complexing agent EDTA plays a crucial role in the process.     

Effect of reaction vessel diameter on sonochemical efficiency and cavitation dynamics

The influence of reaction vessel diameter on the sonochemical yield was investigated by using reaction vessels with five different diameters. It was revealed that the formation of H₂O₂ and chloride ion, from the sonolysis of pure water and 1,2,4-trichlorobenzene aqueous solution, was affected by the reaction vessel diameter. That is, these yields increased as the reaction vessel diameter increased up to ø 90 mm and then decreased over ø 90 mm. From the analyses of the measurement of sonochemiluminescence and the calorimetry, it was suggested that active cavitation bubbles were formed at certain zones. In the case of a larger diameter reaction vessel, it was suggested that bubble nuclei that have not grown up to the resonance size, escaped from the sonication zone to the non-sonication zone and dissolved away. As a result, the number of active cavitation bubbles and the yields of H₂O₂ and chloride ion would decrease in the case of a larger diameter reaction vessel.     

Production of cerium zinc molybdate nano pigment by innovative ultrasound assisted approach

Ultrasound assisted synthesis of yellow rare earth cerium zinc molybdate anticorrosion nanopigment is presented. This new class of pigment is eco-friendly alternatives to lead, cadmium and chromium pigment as these pigments contains carcinogenic species like Cr⁶⁺ which is responsible for human disease. The synthesis of nanosized cerium zinc molybdate was carried out using cerium nitrate, sodium zinc molybdate as a precursor materials by conventional and ultrasound assisted chemical precipitation method without addition of emulsification agent. XRD, FTIR and elemental analysis confirm the formation of cerium zinc molybdate nanoparticles. The conductivity results indicate that conventional synthesis takes longer time, while in sonochemical technique (US), reaction completes within short period of time. Improved solute transfer rate, rapid nucleation, and formation of large number of nuclei are attributed to presence of cavitation. Saturation of the Ce³⁺ ions reaches earlier in case of sonochemical technique which restricts the growth of particles hence smaller size is obtained. The crystallite size of cerium zinc molybdate was found to be 27 nm from XRD analysis.     

Synthesis of tin nanorods via a sonochemical method combined with a polyol process

Metallic tin nanorods were synthesized by a sonochemical method employing the polyol process. In the reaction a solution of SnCl2 in ethylene glycol was exposed to high-intense ultrasound irradiation. The phase and elemental compositions, and thermal properties of the as-synthesized samples were characterized by XRD, EDX, SAED, XPS, DSC, TGA, and BET measurements. The morphologies of the products were further characterized with SEM, TEM, and HRTEM. The results show that crystallized metallic tin nanorods in diameters of 50-100 nm and in lengths of up to 3 microm were synthesized. The nanorods are encapsulated in a thin layer containing Ti and carbon compounds. On the basis of the obtained data, a possible mechanism of the formation of tin nanorods was proposed.     

Sonochemical synthesis and characterization of Co3O4 nanocrystals in the presence of the ionic liquid [EMIM][BF4]

For the first time, a sonochemical process has been used to synthesis cobalt oxide Co₃O₄ nanoflowers and nanorods morphology in the presence of the ionic liquid 1-Ethyl-3-methylimidazolium tetrafluoroborate [EMIM][BF₄] as reaction media and morphology template. Different sonication time periods and different molar ratios of the ionic liquid (IL) were used to investigate their effects on the structural, optical, chemical and magnetic properties of the produced Co₃O₄ nanoparticles. During synthesis process brown powder contains cobalt hydroxide Co(OH)₂ and cobalt oxyhydroxide (Cobalt hydroxide oxide) CoO(OH) was formed, after calcination in air for 4 h at 400 °C a black powder of Co₃O₄ nanoparticles was produced. The produced Co₃O₄ nanoparticles properties were characterized by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), transmission electron microscopy (TEM), FTIR spectroscopy, UV–vis spectroscopy, and Vibrating Sample Magnetometer (VSM). To explain the formation mechanism of Co₃O₄ NPs some investigations were carried on the brown powder before calcination.     

Synthesis and Characterization of Ag@TiO2 Core-shell Nanoparticles and TiO2 Nanobubbles

Ag@TiO₂ core-shell structured particles of nano-size dimensions have been successfully prepared via a one-step way, which has proved quite effective in procuring stable colloids. Transmission electron microscopy (TEM) was employed to characterize the core size and the shell thickness, which typically were 20~40 nm and ~2 nm, respectively. X-ray diffraction (XRD) indicated the existence of silver. Optical absorption dependence on core size and synthetic temperature has been explored by UV–Vis absorption spectroscopy. Finally, the interesting titanium dioxide nanobubbles with silver core leached out by a unique means, were studied, which consequently proved the core-shell structure of the prepared nanoparticles, confirming the TEM observation.     

Ultrasound assisted synthesis of nano-sized lithium cobalt oxide

Nano-sized HT-LiCoO(2) powders were prepared by sonochemical synthesis in an aqueous solution of lithium hydroxide containing cobalt hydroxide at approximately 80 degrees C without any further heat treatment at high temperature. The effects of the LiOH concentration, oxidation conditions, ultrasound irradiation time and temperature on the formation of the nano-sized HT-LiCoO(2) phase were investigated. The formation of the HT-LiCoO(2) phase was confirmed by X-ray diffraction and Raman spectroscopy. The TEM images showed the presence of HT-LiCoO(2) aggregates with a mean particle diameter of approximately 20 nm. The reaction mechanism of the ultrasound assisted synthesis of nano-sized LiCoO(2) was proposed on the basis of the XRD, X-ray absorption spectroscopy analysis and TEM observation of the reaction products taken during the course of the synthesis.