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.     

XPS analysis of sonochemically prepared SbSI ethanogel

This paper, for the first time, presents the results of the X-ray photoelectron spectroscopy (XPS) of the valence band and core levels in sonochemically prepared SbSI ethanogel consisting of nanowires. The XPS spectra were measured with monochromatized Al K_α radiation in the energy range of 0-1400 eV at room temperature. It was found that the sonochemically prepared SbSI ethanogel is a p-type semiconductor. The XPS determined composition of this material suggests the existence of antimony subiodide at surfaces of SbSI nanowires. The chemical shifts in SbSI ethanogel for the Sb, I and S states are reported. Experimentally obtained binding energies are compared with the results reported for single crystals of SbSI.     

Sonochemical growth of antimony sulfoiodide in multiwalled carbon nanotube

This paper presents for the first time the nanocrystalline, semiconducting ferroelectrics antimony sulfoiodide (SbSI) grown in multiwalled carbon nanotubes (CNTs). It was prepared sonochemically using elemental Sb, S and I in the presence of methanol under ultrasonic irradiation (35 kHz, 2.6 W/cm²) at 323 K for 3 h. The CNTs filled with SbSI were characterized by using techniques such as powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, high-resolution transmission electron microscopy, selected area electron diffraction, and optical diffuse reflection spectroscopy. These investigations exhibit that the SbSI filling the CNTs is single crystalline in nature and in the form of nanowires. It has indirect forbidden energy band gap E_gIf = 1.871(1) eV.     

Fabrication and characterization of electrospun orthorhombic InVO4 nanofibers

The novel orthorhombic InVO₄ nanofibers have been successfully synthesized by annealing electrospun precursor fibers. Citric acid was used as a ligand for it could react with metal salts to get a transparent homogeneous precursor solution and homogeneous precursor sol for electrospining. Polyvinyl pyrrolidone (PVP, K-30) was used as a binder and a structure guide reagent because it was one kind of water-soluble polymers. It is easy to gain one-dimensional materials while the viscosity of the citrate/PVP sol was suitable. The structure, morphology and photocatalytic properties of the nanofibers were characterized by X-ray diffraction (XRD), thermogravimetry analysis (TGA), scanning electron microscopy (SEM) analysis, UV-vis spectrophotometer and fluorescence spectrophotometer. The nanofibers calcined at 700 °C were orthorhombic InVO₄ with a width in the range of 30-100 nm and length in micron-grade. This one-dimensional pure orthorhombic InVO₄ had the higher photocatalytic activity under visible light irradiation. The photo-degradation rate of nitrobenzene aqueous solution under visible light reached 69% after 6 h. It is obvious that the orthorhombic InVO₄ nanofibers have a potential application in wastewater-treatment.     

Fragrance release profile from sonochemically prepared protein microsphere containers

Protein microspheres have been prepared by sonicating a mixture of pure fragrant oil (amyl acetate (AA)) with an aqueous protein (bovine serum albumin) solution. The prepared protein spheres are nano- to micrometer sized with an encapsulation efficiency of approx. 97% for the AA present on the surface and inside the BSA capsule. Containers were found stable for more than 6 months when stored sealed at 4 °C and 20 °C. For the release profile measurements, we used a simple, automated and direct method. We continuously weighed the encapsulated microspheres and measured the evaporation rates. The release profiles at 15 °C and 25 °C display two different evaporation rates. The higher rate is the sum of a few evaporation rates, including water molecules, while the slower rate is due to the evaporation of pure AA. The changes in the evaporation rates occur upon the collapse of the container. This event coincides with the full evaporation of water. For morphological characterization we dyed the AA with Nile red, and used SEM, ESEM, Cryo-SEM, light microscopy, and confocal laser scanning microscopy measurements.     

Development of high efficiency nanofilters made of nanofibers

Electrospinning is a fabrication process that uses an electric field to control the deposition of polymer fibers onto a target substrate. This electrostatic processing strategy can be used to fabricate fibrous polymer mats composed of fiber diameters ranging from several microns down to 100 nm or less. In this study, optimized conditions to produce nanofibers using Nylon 6 are investigated and the Nylon 6 nanofilters using nanofibers of 80–200 nm in diameter are designed and evaluated the filtration efficiency and pressure drop across the filter. When the Nylon 6 concentration is 15 wt.%, electrospun fibers have an average diameter of 80 nm, but there are many beads, and the concentration increases to 24 wt.%, the fiber diameter gradually thickens to 200 nm, but there are not any beads. When the spinning distance is small, the thinner nanofibers are produced and the more fibers are collected on the grounded electrode. The filtration efficiency of Nylon 6 nanofilters is 99.993% superior to the commercialized HEPA filter at the face velocity of 5 cm/s using 0.3 μm test particles. Even though the high pressure drops across the nanofilter, they show the potential to have the application of HEPA and ULPA grade high efficiency filter.     

Fabrication of titanium dioxide nanofibers containing hydroxyapatite nanoparticles

In the present study, we introduce titanium dioxide (TiO₂) nanofibers that contain hydroxyapatite (HAp) nanoparticles (NPs) as a result of an electrospinning process. A simple method that does not depend on additional foreign chemicals has been employed to synthesize HAp NPs through calcination of bovine bones. Typically, a colloidal gel consisting of titanium isopropoxide/HAp was prepared to produce nanofibers embedded with solid NPs by electrospinning process. The SEM results confirmed well oriented nanofibers and good dispersion of HAp NPs over the nanofibers. XRD results demonstrated well crystalline feature of both TiO₂ and HAp. Physiochemical aspects of prepared nanofibers were characterized for TEM and TEM-EDS which confirmed nanofibers were well oriented and had good dispersion of HAp NPs. Accordingly, these results strongly recommend the use of obtained nanofiber mats as a future candidate for hard tissue engineering applications.     

Preparation and photoluminescence properties of electrospun nanofibers of C60/PVK

Ultrafine fullerene (C60)/poly(N-vinylcarbazole) (PVK) composite fibers with 1 μm diameter were prepared by electrospinning C60/PVK blend solutions in solvent mixtures of N,N-dimethylformamide (DMF)/toluene. The UV absorption spectra of nanofibers have a similar behavior as observed in the thin films for the same doping condition. It is interesting to observe that the PVK nanofibers have a very strong blue-violet luminescence, while ‘bright spots’ due to C60 can be observed on the C60/PVK fibers under UV irradiation in a fluorescence optical microscope. Compared to the emission spectra of PVK thin films, the photoluminescence of the PVK nanofibers shows a new emission peak at 437 nm. Efficient energy transfer was observed in C60/PVK thin films, as well as in blend nanofibers.     

Electrospinning of complex oxide nanofibers

Electrospinning is a versatile process for drawing fibers of diverse materials including polymers, ceramics, and composites. We demonstrate here its application in the synthesis of complex ceramic oxide materials. The phase formation and morphology of BaTiO₃ nanofibers synthesized via electrospinning is investigated as a function of heat treatment conditions. Fully crystallized BaTiO₃ nanofibers with the perovskite structure are obtained after annealing at 750 °C and show an average grain size of about 30 nm. Tetragonal crystal structure of the fibers is indicated by XRD peak splitting (calculated c/a ratio=1.007), and confirmed by Raman spectroscopy. Furthermore, the advancement in heat treatment of the electrospun fibers yields single crystalline BaTiO₃ nanofibers with 50 nm in diameter and lengths up to 1 μm.     

Piezoelectric and magnetoelectric properties of PVDF/NiFe2O4 based electrospun nanofibers for flexible piezoelectric nanogenerators

In this study, flexible piezoelectric nanogenerators (PNGs) were fabricated using the composite fibers which were prepared by combining polyvinylidene difluoride (PVDF) and nickel ferrite (NiFe₂O₄) nanoparticles (NPs) at a concentration of 1, 3, 5, 7, and 10 wt%. The piezoelectric properties of PNG indicate that the PVDF/NiFe₂O₄ fibers containing NiFe₂O₄ NPs at a concentration of 10 wt% has a higher power efficiency of 5.4% at 20 Hz compared to that of the pure PVDF fibers at 10 Hz, under the same resistive load of 2.5 MΩ. The magnetoelectric properties of PNG show that the PNG with PVDF+7 wt%NiFe₂O₄ supplied the highest electrical power of 0.40 μW under a resistive load of 750KΩ while it reached a maximum voltage value of 17.50 mV at the same load resistive load for a low-level magnetic field of 50 Hz frequency.     

A mathematical model of external electrostatic field of a special collector for electrospinning of nanofibers

This article focuses on the analysis of electrostatic field generated by a special collector consisting of two parallel cylindrical conductors used for electrospinning. Computed values of critical electrical potential obtained by an analytical model are compared with measurements. Here we show that the gap distance between the special collector and a spinning electrode, i.e., a syringe needle, has not substantial effect on the critical potential if the special collector distance from the syringe needle is higher than the gap distance between cylindrical conductors. The presented model is a good analytical approximation of electric field created by the used special collector.     

Modification of surface properties of electrospun polyamide nanofibers by means of a perfluorinated acridine

Polyamide 6 (PA6) nanofibers were prepared from formic acid solutions by using electrospinning technique. The fibers were smooth, defects free and with diameters smaller than 200 nm. Small amounts of a perfluorinated acridine were added as dopant to the feed solution to modify the wettability of the fibers. The effect of doping on the contact angle values is well apparent. The contact angle values go from 50° of pure PA6 to 120° when 6% of acridine is added. A comparison between fibers and films of pure and doped polyamide 6 was carried out in order to determine the effect of morphology on wettability. Thermal annealing near the T_g of the polymer promoted the segregation of the molecules to the surface, reaching contact angles of 131° with smaller amounts (4%) of acridine. The surface segregation was also promoted by time aging.     

Formation of high aspect ratio polyamide-6 nanofibers via electrically induced double layer during electrospinning

In the present study, the formation of high aspect ratio nanofibers in polyamide-6 was investigated as a function of applied voltage ranging from 15 to 25 kV using electrospinning technique. All other experimental parameters were kept constant. The electrospun polyamide-6 nanofibers were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and matrix-assisted laser desorption ionization time-of-flight (MALDI-TOF). FE-SEM images of polyamide-6 nanofibers showed that the diameter of the electrospun fiber was decreased with increasing applied voltage. At the critical applied voltage, the polymer solution was completely ionized to form the dense high aspect ratio nanofibers in between the main nanofibers. The diameter of the polyamide-6 nanofibers was observed to be in the range of 75-110 nm, whereas the high aspect ratio structures consisted of regularly distributed very fine nanofibers with diameters of about 9-28 nm. Trends in fiber diameter and diameter distribution were discussed for the high aspect ratio nanofibers. TEM results revealed that the formation of double layers in polyamide-6 nanofibers and then split-up into ultrafine fibers. The electrically induced double layer in combination with the polyelectrolytic nature of solution is proposed as the suitable mechanisms for the formation of high aspect ratio nanofibers in polyamide-6.     

Short electrospun composite nanofibers: Effects of nanoparticle concentration and surface charge on fiber length

Short composite nanofibers were fabricated by electrospinning polymer/TiO₂ nanoparticle solutions of 13 wt. % cellulose acetate as a polymer under a voltage of 5.5 kV and at a flow rate of 0.1 μL/min, and the nanoparticles could be added in concentrations as high as 50 wt. %. The length of the short composite nanofibers was significantly decreased from 112 to 70 μm by the addition of at least a 5 wt. % concentration of nanoparticles, and it gradually continued to decrease as the nanoparticle concentration was increased. The length of the short composite nanofibers with a low concentration of nanoparticles was affected by the surface charge of the nanoparticles, and negatively charged nanoparticles readily dispersed to the negatively charged polymers in solution, which resulted in an elongation of the fabricated short composite nanofibers.     

Evaluation the pozzolanic reactivity of sonochemically fabricated nano natural pozzolan

Natural pozzolans are appropriate supplementary cementitious materials in cement and concrete industry. A simple sonochemical method was developed to synthesize nanostructures of natural pozzolan. Chemical composition, crystallinity, morphology and reactivity of the natural pozzolan samples were compared before and after the sonochemical process, by using powder X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Thermal Gravimetry and Differential Thermal Analysis (TG/DTA). Compressive strength tests were performed to evaluate the properties of blended cements incorporating nano natural pozzolan. Under optimized conditions, the nano natural pozzolans showed a superior reactivity as compared with the bulk natural pozzolan. Also higher compressive strength was obtained for the cement specimen incorporating nano natural pozzolan.     

Sonochemical preparation of antimony subiodide

The substantiated isolation of the antimony subiodide (Sb₃I) is presented for the first time. It has been prepared using elemental Sb and I in ethanol under ultrasonic irradiation at 323 K. Its composition was characterized using X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray analysis (EDAX). The scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) investigations exhibit that the samples are made up of large quantity of nanoparticles with diameters smaller than 20 nm and single crystalline in nature. The interplanar spacings in Sb₃I that have been determined using powder X-ray diffraction (XRD), selected area electron diffraction (SAED) and HRTEM are very similar. Surprisingly, the registered XRD patterns are identical to the one reported earlier for Sb₄O₅I₂.     

Femtosecond laser machining of electrospun membranes

We demonstrate that a femtosecond laser can be used to machine arbitrary patterns and pattern arrays into free-standing electrospun polycaprolactone (PCL) membranes. We also examine the influence of various laser irradiation settings on the final microstructure of electrospun membranes. A beam fluence of 0.6 J/cm² is used to ablate holes in 100 μm thick PCL membranes. The machined holes have an average diameter of 436 μm and a center-to-center spacing of 1000 μm. Based on these results, the femtosecond ablation of electrospun membranes shows great potential for fabricating a variety of functional tissue scaffolds. This technique will advance scaffold design by providing the ability to rapidly tailor surface morphology, while minimizing and controlling the deformation of the electrospun fibers.     

Crystallization behavior of iron-based amorphous nanoparticles prepared sonochemically

In general, a rapid quenching is required to obtain an amorphous metal. It is known that an intensive ultrasonication generates a very high temperature within cavitation bubbles in a very short moment, which enables a rapid quenching process in a liquid phase synthesis. In this study, the sonochemically-derived “amorphous iron” from Fe(CO)₅ was carefully examined by XRD, TEM, TG-DTA. The product was found to be an amorphous containing a certain amount (∼15%) of volatile component that can be removed by heating in a nitrogen flow. After annealed in the inert atmosphere at 600 °C, cooled down to room temperature, and then exposed in air (oxygen), the sample showed a strong exotherm accompanied by a weight gain. This is due to oxidation of fine metallic iron. Experimental operations of such a reactive material were examined.     

Highly oriented electrospun polycaprolactone micro/nanofibers prepared by a field-controllable electrode and rotating collector

Novel ZnO tetrapod-shaped nanostructures with pearl-necklace-shaped arms were successfully synthesized using mixture of Zn, ZnO, and carbon powder as source. The definite supersaturation ratio provided by Zn, ZnO, and carbon powder was considered as the crucial factor of determining the formation of this kind of structure, and a negative feedback growth model combined with octahedral nucleation mechanism was proposed. Two other comparative experiments were also conducted to study the growth behavior of reagent species under different supersaturation ratios. Our experiments provided a beneficial experimental exploration in controlled growth of nanostructures through modulating supersaturation ratio by source, and these obtained novel nanostructures were also expected to have potential application as functional blocks in nanodevices. Furthermore, the study of photoluminescence indicated that the physical properties were strongly dependent on the crystal structure.     

Preparation of NiZn-ferrite nanofibers by electrospinning for DNA separation

We present the synthesis, magnetic and UV spectrometry of NiZn-ferrite nanofiber. The single phase of spinel ferrite was obtained at 600 °C. The NiZn-ferrite fibers fabricated by an electrospinning process were formed as a polygonal grain growth with firing temperature in fiber matrix. It appeared that the saturation magnetization (M_S) of NiZn-ferrite nanofiber was dependent on Ni/Zn molar ratio which is similar to that of the inverse spinel ferrites. The NiZn-ferrite fibers showed good DNA adsorption efficiency that can be modified and utilized for DNA separation with magnetic nanofiber as a novel material in clinical applications.