Optimization of ultrasonic-assisted approach for synthesizing a highly stable biocompatible bismuth-coated iron oxide nanoparticles using a face-centered central composite design

The incorporation of additional functional groups such as bismuth nanoparticles (Bi NPs) into magnetite nanoparticles (Fe₃O₄ NPs) is critical for their properties modification, stabilization, and multi-functionalization in biomedical applications. In this work, ultrasound has rapidly modified iron oxide (Fe₃O₄) NPs via incorporating their surface through coating with Bi NPs, creating unique Fe₃O₄@Bi composite NPs. The Fe₃O₄@Bi nanocomposites were synthesized and statistically optimized using an ultrasonic probe and response surface methodology (RSM). A face-centered central composite design (FCCD) investigated the effect of preparation settings on the stability, size, and size distribution of the nanocomposite. Based on the numerical desirability function, the optimized preparation parameters that influenced the responses were determined to be 40 ml, 5 ml, and 12 min for Bi concentration, sodium borohydride (SBH) concentration, and sonication time, respectively. It was found that the sonication time was the most influential factor in determining the responses. The predicted values for the zeta potential, hydrodynamic size, and polydispersity index (PDI) at the highest desirability solution (100%) were −45 mV, 122 nm, and 0.257, while their experimental values at the optimal preparation conditions were −47.1 mV, 125 nm, and 0.281, respectively. Dynamic light scattering (DLS) result shows that the ultrasound efficiently stabilized and functionalized Fe₃O₄NPs following modification to Fe₃O₄@Bi NPs, improved the zeta potential value from –33.5 to −47.1 mV, but increased the hydrodynamic size from 98 to 125 nm. Energy dispersive spectroscopy (EDX) validated the elemental compositions and Fourier transform infrared spectroscopy (FTIR) confirmed the presence of Sumac (Rhus coriaria) compounds in the composition of the nanocomposites. The stability and biocompatibility of Fe₃O₄@Bi NPs were improved by using the extract solution of the Sumac edible plant. Other physicochemical results revealed that Fe₃O₄NPs and Fe₃O₄@Bi NPs were crystalline, semi-spherical, and monodisperse with average particle sizes of 11.7 nm and 19.5 nm, while their saturation magnetization (Ms) values were found to be 132.33 emu/g and 92.192 emu/g, respectively. In vitro cytotoxicity of Fe₃O₄@Bi NPs on the HEK-293 cells was dose- and time-dependent. Based on our findings, the sonochemical approach efficiently produced (and RSM accurately optimized) an extremely stable, homogeneous, and biocompatible Fe₃O₄@Bi NPs with multifunctional potential for various biomedical applications.     

Template-free sonochemical synthesis of flower-like ZnO nanostructures

Flower-like ZnO nanostructures have been successfully synthesized via a facile and template-free sonochemical method, using zinc acetate and potassium hydroxide as reactants only. The as-synthesized flower-like ZnO nanostructures were composed of nanorods with the width of ∼300–400 nm$\sim 300\text{–}400\text{nm}$ and the length of ∼2–3 μm$\sim 2\text{–}3\text{μm}$. The structures, morphologies and optical properties of the as-prepared products were characterized by X-ray diffraction, scanning electron microscope, transmission electron microscopy, UV-Vis spectrophotometry and Raman-scattering spectroscopy. A plausible formation mechanism of flower-like ZnO nanostructures was studied by SEM which monitors an intermediate morphology transformation of the product at the different ultrasonic time (t=80,90,95,105, and 120 min$t=80,90,95,105\text{, and}120\text{min}$).     

One-step simple sonochemical fabrication and photocatalytic properties of Cu2O–rGO composites

An easy, one-step synthesis of Cu₂O–reduced graphene composites (Cu₂O–rGO) was developed using a simple sonochemical route without any surfactants or templates. The morphology and structure of the Cu₂O–rGO composites were characterised using techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The results indicated that the Cu₂O sphere is approximately 200 nm in diameter and composed of small Cu₂O particles approximately 20 nm in diameter. The morphology and composition of the Cu₂O–rGO composites could be well controlled by simply changing the mole ratio of the reactants under ultrasonic irradiation. The Cu₂O–rGO composites displayed better photocatalytic performance for the degradation of methyl orange (MO) than pure Cu₂O spheres, which may have potential applications in water treatment, sensors, and energy storage.     

Sonochemical syntheses of a new fibrous-like nano-scale manganese(II) coordination supramolecular compound; precursor for the fabrication of octahedral-like Mn3O4 nano-structure

Nanoparticles of a new three-dimensional Mn(II) coordination supramolecular compound, [Mn(L)₂(H₂O)₂] (1), (L⁻ = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analyses. Structural determination of compound 1 reveals the Mn(II) ion is six coordinated, bonded to two nitrogen atoms, two oxygen atoms from the L⁻ ligand and two water molecules. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied and shows that low concentrations of initial reagents decreased particles size and also leaded to fibrous-like nanostructures morphology. Mn₃O₄ nano-structure with an octahedral-like morphology were simply synthesized by solid-state transformation of compound 1 at 650 °C.     

Nanocrystals of XTiO3 (X = Ba,Sr, Ni,BaxTi1−x) materials obtained through a rapid one-step methodology at 50 °C

Titanate-based perovskite (XTiO₃; Ba, Sr, Ni, Ba_0.6Sr_0.4) nanocrystals were synthesized through a unified sonochemical methodology based on the reaction between XCl₂ and TiCl₄. The effects of the preparation conditions such as ultrasonication time and ultrasonication temperature were studied. XTiO₃ nanocrystals were characterized by field-emission scanning electron microscopy (FE-SEM), X-Ray diffractometry and high-resolution transmission electron microscopy techniques. XTiO₃ nanocrystals were synthesized at a relatively low temperature of 50 °C while were free from any by-product such as XCO₃ (carbonate by-products). Characterization of the morphological characteristics and particle size distribution of the obtained powders indicated that the powder products consist of somewhat regularly shaped and relatively spherical particles with a narrow size distribution. The method described here, is simple, rapid, cost-effective and useful for large-scale production purposes.     

Enhancing the formation of tetragonal phase in perovskite nanocrystals using an ultrasound assisted wet chemical method

Synthesis of highly-pure tetragonal perovskite nanocrystals is the key challenge facing the development of new electronic devices. Our results have indicated that ultrasonication is able in enhancing the formation of tetragonal phase in perovskite nanocrystals. In the current research, multicationic oxide perovskite (ATiO₃; A: Ba, Sr, Ba_0.6Sr_0.4) nanopowders are synthesized successfully by a general methodology without a calcination step. The method is able to synthesize high-purity nanoscale ATiO₃ (BaTiO₃, SrTiO₃, Ba_0.6Sr_0.4TiO₃) with tetragonal symmetry at a lower temperature and in a shorter time span in contrast to the literature. To reach an in-depth understanding of the scientific basis of the proposed methodology, in-detail analysis was carried out via XRD, FTIR, FT-Raman, FE-SEM and HR-TEM. The effects of the sonication time and sonication (bath) temperature on the tetragonality of nanoscale products were examined. Furthermore, Raman spectroscopy provides clear evidence for local tetragonal symmetries, in particular when a band is observed at 310 cm⁻¹.     

A simple sonochemical approach for synthesis and characterization of Zn2SiO4 nanostructures

Zn₂SiO₄ nanoparticles have been successfully prepared via a simple sonochemical method, for the first time. The effect of various parameters including ultrasonic power, ultrasonic irradiation time and different surfactants were investigated to reach optimum condition. The as-prepared nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmittance electron microscopy (TEM), Fourier transform infrared (FT-IR) spectra and energy dispersive X-ray microanalysis (EDX). The photocatalytic activity of Zn₂SiO₄ nano and bulk structures were compared by degradation of anionic dye methyl orange in aqueous solution under UV-light irradiation. Moreover, the cyclic voltammetry analysis of Zn₂SiO₄ nano and bulk structures were investigated.     

A novel approach to preparing magnetic protein microspheres with core-shell structure

Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method. The microspheres are composed of the oleic acid and undecylenic acid modified Fe₃O₄ cores and coated with globular bovine serum albumin (BSA). Under an optimized condition, up to 57.8 wt% of approximately 10 nm superparamagnetic Fe₃O₄ nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides of the abundant functional groups. The possible formation mechanism of magnetic microspheres was discussed in detail.     

Effects of Solvent and Reaction Time in Sonochemical Synthesis of Cadmium(II) Compounds and Use them as Template for Synthesis of Cadmium(II) Oxide Nano Structures

Abstract . A cadmium(II) zero-dimensional supramolecular compound [Cd(L)₂(I)₂] ( 1 ), {L = 2-picolylamine}, was fabricated by branch tube and sonochemical irradiation techniques. Regardless of the method utilized, the same crystallographic structure is obtained for the complex. To investigate the effects of reaction time and solvent on the creation of [Cd(L)₂(I)₂] ( 1 ) supramolecule compound, certain tests were designed and four specimens of 1 were fabricated through sonochemical process. Less reaction time led to the creation of smaller particles with mixed morphologies. To prepare cadmium(II) oxide micro-crystals via calcination, four samples were utilized as new precursors. Micro- and nano-sphere of cadmium(II) oxide could be fabricated from 1. The morphology and structure of micro- and nano-crystals were identified by using Scanning Electron Microscopy (SEM), IR spectroscopy, and X-ray powder diffraction (XRD).