Scaling up the fabrication of wafer-scale Ni-MoS2/WS2 nanocomposite moulds using novel intermittent ultrasonic-assisted dual-bath micro-electroforming

In the scale-up fabrication process for electroformed Ni-MoS₂/WS₂ composite moulds, the formulation of nanosheets is critical, since the size, charge, and their distribution can largely affect the hardness, surface morphology and tribological properties of the moulds. Additionally, the long-term dispersion of hydrophobic MoS₂/WS₂ nanosheets in a nickel sulphamate solution is problematic. In this work, we studied the effect of ultrasonic power, processing time, surfactant types and concentrations on the properties of nanosheets to elaborate their dispersion mechanism and control their size and surface charge in divalent nickel electrolyte. The formulation of MoS₂/WS₂ nanosheets was optimized for effective electrodeposition along with nickel ions. A novel strategy of intermittent ultrasonication in the dual bath was proposed to resolve the problem of long-term dispersion, overheating, and deterioration of 2D material deposition under direct ultrasonication. Such strategy was then validated by electroforming 4-inch wafer-scale Ni-MoS₂/WS₂ nanocomposite moulds. The results indicated that the 2D materials were successfully co-deposited into composite moulds without any defects, along with the mould microhardness increasing by ∼2.8 times, the coefficient of friction reducing by two times against polymer materials, and the tool life increasing up to 8 times. This novel strategy will contribute to the industrial manufacturing of 2D material nanocomposites under ultrasonication process.     

Anti-solvent precipitation for the preparation of nobiletin nano-particles under ultrasonication-cis/reverse homogenization

In order to address the issue of nobiletin's limited bioavailability, nobiletin nanoparticles (NNP) were created for the first time in this research employing an anti-solvent under ultrasonication-cis/reverse homogenization. Dimethyl sulfoxide (DMSO) was used as the solvent and deionized water as the anti-solvent to create the nobiletin solution. The optimal surfactant dose of surfactant dose of 0.43%; an ultrasonic period of 8.1 min, ultrasonic at a temperature of 64 °C and a solution concentration of 8.33 mg/mL, the method was optimized to obtain the minimum NNP diameter of 199.89 ± 0.02 nm. A dual optimization process of response surface PBD and BBD was used to minimize the size of HNP particles. Additionally, scanning electron microscopy revealed that the specific surface area of the NNP dramatically increased with the reduction of NNP particle size, and dissolving studies indicated the solubility and dissolution studies showed that NNP had substantially greater solubility and dissolution rates than raw nobiletin per unit time; as a result, the NNP produced by anti-solvent precipitation with a twofold homogenization system supported by ultrasound had a realistic potential for growth.     

Ultrasonically activated reduction of substituted nitrobenzenes to corresponding N-arylhydroxylamines

Arylhydroxylamines can be obtained by reduction of the corresponding nitroaromatic compounds. We report here an efficient preparation of arylhydroxylamines by a controlled reduction of nitro compounds using zinc metal and ammonium chloride under ultrasonic activation in very short reaction times.     

PET-SWNT nanocomposites through ultrasound assisted dissolution-evaporation

Poly(ethylene terephthalate) (PET) based nanocomposites have been prepared with single walled carbon nanotubes (SWNTs) through an ultrasound assisted dissolution-evaporation method. Differential scanning calorimetry studies showed that SWNTs nucleate crystallization in PET at weight fractions as low as 0.3%, as the nanocomposite melt crystallized during cooling at temperature 24 °C higher than neat PET of identical molecular weight. Isothermal crystallization studies also revealed that SWNTs significantly accelerate the crystallization process. Mechanical properties of the PET-SWNT nanocomposites improved as compared to neat PET indicating the effective reinforcement provided by nanotubes in the polymer matrix. Electrical conductivity measurements on the nanocomposite films showed that SWNTs at concentrations exceeding 1 wt% in the PET matrix result in electrical percolation. Comparison of crystallization, conductivity and transmission electron microscopy studies revealed that ultrasound assisted dissolution-evaporation method enables more effective dispersion of SWNTs in the PET matrix as compared to the melt compounding method.     

Ultrasound-assisted rapid and efficient synthesis of propargylamines

Ultrasound was used for the addition of metal acetylides to in situ generated imines to generate propargylamines in good to excellent yields using copper iodide in water at ambient temperature. This process is an efficient alternative to traditional heated reactions. A variety of aldehydes and amines were used for this reaction.     

Ultrasound-promoted a green protocol for the synthesis of 2,4-diarylthiazoles under ambient temperature in [bmim]BF4

A mild, efficient, facile and eco-friendly procedure for the synthesis of 2,4-diarylthiazoles from arylthioamides and α-bromoacetophenones in 1-n-butyl-3-methylimidazolium tetrafluoroborate as a “green” media under ultrasound irradiation at room temperature is described. It is interesting to mention that only one product was obtained when two different α-bromoacetophenones were reacted with 1,3-phenyl dithioamide as the substrate. Work-up is very simple and there is no need to purify the product. A recycling study confirmed that the ionic liquid can be reused multiple times without a significant loss in its activity.     

Sustained release formulations of citronella oil nanoemulsion using cavitational techniques

Nanoemulsion synthesis has proven to be an effective way for transportation of immobile, insoluble bioactive compounds. Citronella Oil (lemongrass oil), a natural plant extract, can be used as a mosquito repellent and has less harmful effects compared to its available market counterpart DEET (N, N-Diethyl-meta-toluamide). Nanoemulsion of citronella oil in water was prepared using cavitation-assisted techniques while investigating the effect of system parameters like HLB (Hydrophilic Lipophilic Balance), surfactant concentration, input energy density and mode of power input on emulsion quality. The present work also examines the effect of emulsification on release rate to understand the relationship between droplet size and the release rate. Minimum droplet size (60 nm) of the emulsion was obtained at HLB of 14, S/O¹ ratio of 1.0, ultrasound amplitude of 50% and irradiation time of 5 min. This study revealed that hydrodynamic cavitation-assisted emulsification is more energy efficient compared to ultrasonic emulsification. It was also found that the release rate of nanoemulsion enhanced as the droplet size of emulsion reduced.     

Optimization and characterization of ultrasound assisted preparation of curcumin-loaded solid lipid nanoparticles: Application of central composite design,thermal analysis and X-ray diffraction techniques

This study is devoted to preparation of novel solid lipid nanoparticles (SLNs) for the encapsulation of curcumin which is produced by micro-emulsion and ultrasonication using stearic acid and tripalmitin as solid lipids, tween80 and span80 as surfactants. The relation between particle size and entrapment efficiency of the produced SLNs was operated by central composite design (CCD) under response likes surface method (RSM). The variables including the ratio of lipids (X₁), the ratio of surfactants (X₂), drug/lipid ratio (X₃), time of sonication (X₄) and time of homogenization (X₅). Particle size and entrapment efficiency of the loaded curcumin was justified according to the minimum particle size and maximum entrapment efficiency. The curcumin loaded SLNs presented fairly spherical shape with the mean diameter and entrapment efficiency of 112.0 ± 2.6 nm and 98.7 ± 0.3%, respectively. The optimized SLNs were characterized by X-ray diffraction analysis (XRD), differential scanning calorimetry (DSC), photon correlation spectroscopy (PCS) and field emission scanning electron microscopy (FESEM). The drug release profile of the optimal formulated material was examined in aqueous media and almost 30% of the curcumin loaded in SLNs was gradually released during 48 h, which reveals efficient prolonged release of the drug.     

Formulation development and evaluation of metronidazole magnetic nanosuspension as a magnetic-targeted and polymeric-controlled drug delivery system

A nanosuspension of magnetically tagged metronidazole was developed by the solvent displacement method coupled with ultrasonication and was evaluated for its physicochemical properties. The drug release from metronidazole magnetic nanosuspension at pH 1.2 and 7.0 shows maximum correlation coefficient for zero order and Higuchi model, respectively. The anthelmintic activity of the formulated metronidazole magnetic nanosuspension was evaluated on Indian earthworms (Pheretima poi). Metronidazole magnetic nanosuspension at a dose of 10 and 50 mg/ml shortened by 31% and 34%, respectively, the mean time to death of the earthworms when compared against a non-magnetic metronidazole suspension. Thus, the developed metronidazole magnetic nanosuspension showed potent, controlled and targeted drug action and might be a good therapeutic avenue in combating infectious GI disorders.