Application of high-frequency ultrasound standing waves for the recovery of lipids from high-fat dairy effluent

Effect of high-frequency ultrasonication was examined on wastewater of a cheese manufacturing plant. Tests were carried out at two frequencies (500 kHz and 1 MHz) and two temperatures (22 and 40 °C). Samples were subjected to different energy densities; 7.5, 30.2, 60.5 and 121.0 J/mL at 500 kHz and 7.9, 31.7, 63.4 and 126.8 J/mL at 1 MHz to observe the creaming and recovery of lipid. These energy densities correspond to 30, 120, 240 and 480 s of sonication. Sonication was performed using a single plate transducer and reflector system at 40 W to create standing wave to coalesce and flocculate lipid globules. Recovery was higher at 40 °C after 480 s of sonication at both frequencies (77% at 500 kHz and 75% at 1 MHz). The lowest recovery of 47% was observed at 500 kHz and 22 °C at all applied energy densities. Changes in particle size and turbidity in the bottom aliquot indicated that high-frequency ultrasound caused coagulation and aggregation and settling of colloidal particles. Increase in particle size was observed to be highest at 1 MHz, 40 °C and 480 s of sonication. These results confirm that high-frequency ultrasound standing wave technology can be used to recover lipid from high-lipid dairy wastewater including that from cheese manufacturing.     

Improved direct synthesis of TiO2 catalyst using sonication and its application for the desulfurization of thiophene

TiO₂ catalyst was synthesized in the presence of ultrasound (ultrasonic horn at 20 kHz frequency and 70% duty cycle) at different power (80 W to 120 W) and durations as well as surfactant concentration with an objective of establishing best conditions for achieving lowest particle size of the photocatalyst. Detailed characterization in terms of crystal phase, crystallinity, functional groups and morphology of the photocatalyst has been performed using SEM, XRD and FTIR analysis. It was demonstrated that sonication significantly reduced the particle size with high degree of sphericity and homogeneity as compared to conventionally synthesized TiO₂ with similar crystallinity in both cases. The catalytic performance was subsequently evaluated for the deep desulfurization of thiophene. Different desulfurization approaches including individual US (ultrasonic horn at 20 kHz frequency, 110 W power and 70% duty cycle) and UV irradiations, US/UV, US/UV/H₂O₂, US/UV/TiO₂ and US/UV/H₂O₂/TiO₂ were applied to evaluate the catalytic activity. The best approach was demonstrated as US/UV/H₂O₂/TiO₂ and also activity of catalyst synthesized using ultrasound was much better compared to conventionally synthesized catalyst. The studies related to different model solvents demonstrated lowest reactivity for toluene whereas n-hexane and n-octane resulted in complete desulfurization in 60 min and 50 min treatment respectively. The desulfurization followed pseudo first order reaction kinetics irrespective of the solvent used. Overall the work clearly demonstrated the efficacy of ultrasound in improving the catalyst synthesis as well as desulfurization of thiophene.     

Impact of sonochemical synthesis condition on the structural and physical properties of MnFe2O4 spinel ferrite nanoparticles

Herein, we report sonochemical synthesis of MnFe₂O₄ spinel ferrite nanoparticles using UZ SONOPULS HD 2070 Ultrasonic homogenizer (frequency: 20 kHz and power: 70 W). The sonication time and percentage amplitude of ultrasonic power input cause appreciable changes in the structural, cation distribution and physical properties of MnFe₂O₄ nanoparticles. The average crystallite size of synthesized MnFe₂O₄ nanoparticles was increased with increase of sonication time and percentage amplitude of ultrasonic power input. The occupational formula by X-ray photoelectron spectroscopy for prepared spinel ferrite nanoparticles was (Mn_0.29Fe_0.42)[Mn_0.71Fe_1.58]O₄ and (Mn_0.28Fe_0.54) [Mn_0.72Fe_1.46]O₄ at sonication time 20 min and 80 min, respectively. The value of the saturation magnetization was increased from 1.9 emu/g to 52.5 emu/g with increase of sonication time 20 min to 80 min at constant 50% amplitude of ultrasonic power input, whereas, it was increased from 30.2 emu/g to 59.4 emu/g with increase of the percentage amplitude of ultrasonic power input at constant sonication time 60 min. The highest value of dielectric constant (ε′) was 499 at 1 kHz for nanoparticles at sonication time 20 min, whereas, ac conductivity was 368 × 10⁻⁹ S/cm at 1 kHz for spinel ferrite nanoparticles at sonication time 20 min. The demonstrated controllable physical characteristics over sonication time and percentage amplitude of ultrasonic power input are a key step to design spinel ferrite material of desired properties for specific application. The investigation of microwave operating frequency suggest that these prepared spinel ferrite nanoparticles are potential candidate for fabrication of devices at high frequency applications.     

Effects of multi-frequency ultrasound on physicochemical properties,structural characteristics of gluten protein and the quality of noodle

In this study, the influence of multi-frequency ultrasound irradiation on the functional properties and structural characteristics of gluten, as well as the textural and cooking characteristics of the noodles were investigated. Results showed that the textural and cooking characteristics of noodles that contain less gluten pretreated by multi-frequency ultrasonic were ultrasonic frequency dependent. Moreover, the noodles that contain a smaller amount of sonicated gluten could achieve the textural and cooking quality of commercial noodles. There was no significant difference in the cooking and texture characteristics between commercial noodles and noodles with 12%, 11%, and 10% gluten pretreated by single-frequency (40 kHz), dual-frequency (28/40 kHz), and triple-frequency sonication (28/40/80 kHz), respectively. Furthermore, the cavitation efficiency of triple-frequency ultrasound was greater than that of dual-frequency and single-frequency. As the number of ultrasonic frequencies increased, the solubility, water holding capacity and oil holding capacity of gluten increased significantly (p < 0.05), and the particle size was reduced from 197.93 ± 5.28 nm to 110.15 ± 2.61 nm. Furthermore, compared to the control group (untreated), the UV absorption and fluorescence intensity of the gluten treated by multi-frequency ultrasonication increased. The surface hydrophobicity of gluten increased from 8159.1 ± 195.87 (untreated) to 11621.5 ± 379.72 (28/40/80 kHz). Raman spectroscopy showed that the α-helix content of all sonicated gluten protein samples decreased after sonication, while the β-sheet and β-turn content increased, and tryptophan and tyrosine residues were exposed. Through scanning electron microscope (SEM) analysis, the gluten protein network structure after ultrasonic treatment was loose, and the pore size of the gluten protein network increased from about 10 μm (untreated) to about 26 μm (28/40/80 kHz). This work elucidated the effect of ultrasonic frequency on the performance of gluten, indicating that with increasing frequency combination increases, the ultrasound effect became more pronounced and protein unfolding increased, thereby impacting the functional properties and the quality of the final product. This study provided a theoretical basis for the application of multi-frequency ultrasound technology in the modification of gluten protein and noodle processing.     

Response surface methodology for optimization of cinnamon essential oil nanoemulsion with improved stability and antifungal activity

The optimum formulation and ultrasonic condition for fabrication of cinnamon essential oil (CEO) nanoemulsion were determined using Response Surface Methodology (RSM). The CEO nanoemulsions were formed using an ultrasonic bath (43 kHz at power output of 210 W) and an ultrasonic probe (24 kHz at power of 400 W). Probe ultrasonication outperformed bath ultrasonication since it produced nanoemulsions with smaller droplet size, narrower size distribution as measured using polydispersity index (PDI), and higher viscosity. The influences of sonication time of 180.23–351.77 s, temperature of 4.82–45.18 °C, and Tween® 80 concentration of 1–3% w/w on the droplet size, PDI, and viscosity were investigated using RSM based on Box-Behnken design (BBD). The RSM revealed that the sonication time of 266 s, temperature of 4.82 °C, and Tween® 80 of 3% w/w produced the optimum CEO nanoemulsion with droplet size of 65.98 nm, PDI of 0.15, and viscosity of 1.67 mPa.s. Moreover, the optimum nanoemulsion had good stability in terms of droplet size and PDI when storing at 4, 30, and 45 °C for 90 days. The antifungal activity of the optimum CEO nanoemulsion was then investigated against Aspergillus niger, Rhizopus arrhizus, Penicillium sp., and Colletotrichum gloeosporioides in comparison to CEO coarse emulsion. The results showed that the CEO nanoemulsion had better antifungal activity than coarse emulsion of CEO.     

Dual-frequency multi-angle ultrasonic processing technology and its real-time monitoring on physicochemical properties of raw soymilk and soybean protein

To improve the soybean protein content (SPC), flavor and quality of soymilk, the effects of dual-frequency ultrasound at different angles (40 + 20 kHz 0°, 40 + 20 kHz 30°, 40 + 20 kHz 45°) on physicochemical properties and soybean protein (SP) structure of raw soymilk were mainly studied and compared with the conventional single-frequency (40 kHz, 20 kHz) ultrasound. Furthermore, the intensity of the ultrasonic field in real-time was monitored via the oscilloscope and spectrum analyzer. The results showed that 40 + 20 kHz 45° treatment significantly increased SPC. The ultrasonic field intensity of 40 + 20 kHz 0° treatment was the largest (8.727 × 10⁴ W/m²) and its distribution was the most uniform. The emulsifying stability of SP reached the peak value (233.80 min), and SP also had the largest particle size and excellent thermal stability. The protein solubility of 40 + 20 kHz 30° treatment attained peak value of 87.09%. 20 kHz treatment significantly affected the flavor of okara. The whiteness and brightness of raw soymilk treated with 40 kHz were the highest and the system was stable. Hence, the action mode of ultrasonic technology can be deeply explored and the feasibility for improving the quality of soymilk can be achieved.     

Obtaining Ca(H2PO4)2·H2O,monocalcium phosphate monohydrate,via monetite from brushite by using sonication

Brushite was synthesized by precipitation of calcium chloride (CaCl₂) and sodium phosphate monobasic (Na₂HPO₄) dried in vacuum and monetite was obtained from this brushite by sonication with a frequency of 90 kHz at 500 W for 90 min. Monetite itself was also transformed in Ca(H₂PO₄)₂·H₂O, monocalcium phosphate monohydrate (MCPM), by sonication with a frequency of 90 kHz at 500 W for 60 min followed by lyophilization. The MCPM was sonicated and lyophilized by three times more until reach over 240 min, but any other phase transformation was observed. All these phase transformations were analyzed by X-ray diffraction (XRD) and infrared spectroscopy (FTIR). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated a grain size of about 200 nm in all the samples. The morphology observed was a corn-flake-like grain for brushite, a pseudo-needle-like grains for monetite, and lamellar-like grains for MCPM.     

A fundamental study on the degradation of paracetamol under single- and dual-frequency ultrasound

The degradation of paracetamol, a widely found emerging pharmaceutical contaminant, was investigated under a wide range of single-frequency and dual-frequency ultrasonic irradiations. For single-frequency ultrasonic irradiation, plate transducers of 22, 98, 200, 300, 400, 500, 760, 850, 1000, and 2000 kHz were employed and for dual-frequency ultrasonic irradiation, the plate transducers were coupled with a 20 kHz ultrasonic horn in opposing configuration. The sonochemical activity was quantified using two dosimetry methods to measure the yield of HO• and H₂O₂ separately, as well as sonochemiluminescence measurement. Moreover, the severity of the bubble collapses as well as the spatial and size distribution of the cavitation bubbles were evaluated via sonoluminescence measurement. The paracetamol degradation rate was maximised at 850 kHz, in both single and dual-frequency ultrasonic irradiation. A synergistic index higher than 1 was observed for all degrading frequencies (200 – 1000 kHz) under dual-frequency ultrasound irradiation, showing the capability of dual-frequency system for enhancing pollutant degradation. A comparison of the results of degradation, dosimetry, and sonoluminescence intensity measurement revealed the stronger dependency of the degradation on the yield of HO• for both single and dual-frequency systems, which confirms degradation by HO• as the main removal mechanism. However, an enhanced degradation for frequencies higher than 500 kHz was observed despite a lower HO• yield, which could be attributed to the improved mass transfer of hydrophilic compounds at higher frequencies. The sonoluminescence intensity measurements showed that applying dual-frequency ultrasonic irradiation for 200 and 400 kHz made the bubbles larger and less uniform in size, with a portion of which not contributing to the yield of reactive oxidant species, whereas for the rest of the frequencies, dual-frequency ultrasound irradiation made the cavitation bubbles smaller and more uniform, resulting in a linear correlation between the overall sonoluminescence intensity and the yield of reactive oxidant species.     

Comparison of Eu(NO<Subscript>3</Subscript>)<Subscript>3</Subscript> and Eu(acac)<Subscript>3</Subscript> precursors for doping luminescent silica nanoparticles

In this study, we report the comparison between Eu³⁺-doped silica nanoparticles synthesized by Stöber method using Eu(NO₃)₃ or Eu(acac)₃ as precursors. The impact of different europium species on the properties of the final silica nanospheres is investigated in details in terms of size, morphology, reachable doping amount, and luminescence efficiency. Moreover, the results obtained for different thermal treatments are presented and discussed. It is shown that the organic complex modify the silica growing process, leading to bigger and irregular nanoparticles (500–800 nm) with respect to the perfectly spherical ones (400 nm) obtained by the nitrate salt, but their luminescence intensity and lifetime is significantly higher when 800–900 °C annealing is performed.     

Dual frequency cavitation event sensor with iodide dosimeter

The inertial cavitation activity depends on the sonication parameters. The purpose of this work is development of dual frequency inertial cavitation meter for therapeutic applications of ultrasound waves. In this study, the chemical effects of sonication parameters in dual frequency sonication (40 kHz and 1 MHz) were investigated in the progressive wave mode using iodide dosimetry. For this purpose, efficacy of different exposure parameters such as intensity, sonication duration, sonication mode, duty factor and net ultrasound energy on the inertial cavitation activity have been studied. To quantify cavitational effects, the KI dosimeter solution was sonicated and its absorbance at a wavelength of 350 nm was measured. The absorbance values in continuous sonication mode was significantly higher than the absorbance corresponding to the pulsed mode having duty factors of 20–80% (p < 0.05). Among different combination modes (1 MHz_100% + 40 kHz_100%, 1 MHz_100% + 40 kHz_80%, 1 MHz_80% + 40 kHz_100%, 1 MHz_80% + 40 kHz_80%), the continuous mode for dual frequency sonication is more effective than other combinations (p < 0.05). The absorbance for this combined dual frequency mode was about 1.8 times higher than that obtained from the algebraic summation of single frequency sonications. It is believed that the optimization of dual frequency sonication parameters at low-level intensity (<3 W/cm²) by optically assisted cavitation event sensor can be useful for ultrasonic treatments.     

High yield synthesis of Ni-BTC metal–organic framework with ultrasonic irradiation: Role of polar aprotic DMF solvent

Nickel based porous solid was synthesized with 20 kHz ultrasonic irradiation. The reaction of Ni(II) nitrate hexahydrate with 1,3,5-benzene tricarboxylic acid in N,N-Dimethylformamide (DMF) as the sole solvent under ultrasonic radiation produced porous Ni-BTC MOF. Choice of correct solvent for the ultrasonic treatment was proven important. The effect of varying ultrasonic powers (40%, 60% and 80% of 750 W) along with different temperature conditions (50 °C, 60 °C, 70 °C and 80 °C) influenced the respective yield. A very high yield of 88% Ni-BTC MOF was obtained from 80% ultrasonic power at 60 °C. BET surface areas of the MOF crystals measured by N₂ gas adsorption isotherms were in the range of 960–1000 m²/g.     

Ultrasonic pretreatment of corn slurry for saccharification: A comparison of batch and continuous systems

The effects of ultrasound on corn slurry saccharification yield and particle size distribution was studied in both batch and continuous-flow ultrasonic systems operating at a frequency of 20 kHz. Ground corn slurry (28% w/v) was prepared and sonicated in batches at various amplitudes (192–320 μm_{peak-to-peak (p–p)}) for 20 or 40 s using a catenoidal horn. Continuous flow experiments were conducted by pumping corn slurry at various flow rates (10–28 l/min) through an ultrasonic reactor at constant amplitude of 12 μm_p–p. The reactor was equipped with a donut shaped horn. After ultrasonic treatment, commercial alpha- and gluco-amylases (STARGEN^TM 001) were added to the samples, and liquefaction and saccharification proceeded for 3 h. The sonicated samples were found to yield 2–3 times more reducing sugars than unsonicated controls. Although the continuous flow treatments released less reducing sugar compared to the batch systems, the continuous flow process was more energy efficient. The reduction of particle size due to sonication was approximately proportional to the dissipated ultrasonic energy regardless of the type of system used. Scanning electron microscopy (SEM) images were also used to observe the disruption of corn particles after sonication. Overall, the study suggests that both batch and continuous ultrasonication enhanced saccharification yields and reduced the particle size of corn slurry. However, due to the large volume involve in full scale processes, an ultrasonic continuous system is recommended.     

Electron paramagnetic resonance of sonicated powder suspensions in organic solvents

The chemical effects of the acoustic cavitation generated by ultrasound translates into the production of highly reactive radicals. Acoustic cavitation is widely explored in aqueous solutions but it remains poorly studied in organic liquids and in particular in liquid/solid media. However, several heterogeneous catalysis reactions take place in organic solvents.Thus, we sonicated trimethylene glycol and propylene glycol in the presence of silica particles (SiO₂) of different sizes (5–15 nm, 0.2–0.3 µm, 12–26 µm) and amounts (0.5 wt% and 3 wt%) at an ultrasound frequency of 20 kHz to quantify the radicals generated. The spin trap 5,5-dimethyl-1-pyrrolin–N-oxide (DMPO) was used to trap the generated radicals for study by electron paramagnetic resonance (EPR) spectroscopy. We identified the trapped radical as the hydroxyalkyl radical adduct of DMPO, and we quantified it using stable radical 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) as a quantitation standard. The concentration of DMPO spin adducts in solutions containing silica size 12–26 µm was higher than the solution without particles. The presence of these particles increased the concentration of the acoustically generated radicals by a factor of 1.5 (29 µM for 0.5 wt% of SiO₂ size 12–26 µm vs 19 µM for 0 wt%, after 60 min of sonication). Ultrasound produced fewest radicals in solutions with the smallest particles; the concentration of radical adducts was highest for SiO₂ particle size 12–26 µm at 0.5 wt% loading, reaching 29 µM after 60 min sonication. Ultrasound power of 50.6 W produced more radicals than 24.7 W (23 µM and 18 µM, respectively, at 30 min sonication). Increased temperature during sonication generated more radical adducts in the medium (26 µM at 75 °C and 18 µM at 61 °C after 30 min sonication). Acoustic cavitation, in the presence of silica, increased the production of radical species in the studied organic medium.     

Synergistic effect of sonication on photocatalytic oxidation of pharmaceutical drug carbamazepine

Photocatalytic, sono-photocatalytic oxidation of pharmaceutical drug of carbamazepine was successfully carried out using Ag/AgCl supported BiVO₄ catalyst. For this purpose, firstly, photocatalytic oxidation was optimized by central composite design methodology and then synergistic effect of sonication was investigated. Low frequency (20 kHz) probe type and high frequency (850 kHz) plate type sonication at pulse and continuous mode were studied to degrade the carbamazepine (CBZ) containing wastewater. Pulse duties of 1:5 and 5:1 (on : off) were tested using the high frequency sonication system in the sono-photocatalytic oxidation of CBZ. The effects of frequency, power density measured from calorimetry by changing amplitudes were discussed in the sono-photocatalytic oxidation of CBZ. Complete carbamazepine removal was achieved at the optimum conditions of 5 ppm CBZ initial concentration with 1.5 g/L of catalysts loading and at an alkaline pH of 10 at the end of 4 h of photocatalytic reaction under visible LED light irradiation. Both low frequency and high frequency sonication systems caused an increase in photocatalytic efficiency in a shorter treatment time of 60 min. CBZ removal increased from 44% to 65.42% in low frequency sonication of 20 kHz at the amplitude of 20% (0.15 W/mL power density). In the case of high frequency ultrasonic system (850 kHz), CBZ removal increased significantly from 44% to 89.5 % at 75% amplitude (0.12 W/mL power density) within 60 min of reaction. Continuous mode sonication was observed to be more effective than that of pulse mode sonication not only for degradation efficiency and also for electrical energy consumption needed to degrade CBZ. Sono-catalytic oxidation was also conducted with simulated wastewater that contains SO₄^2-, CO₃^2–, NO^3–, Cl^- anions and natural organic component of fulvic acid. The CBZ degradation was inhibited slightly in the presence of NO₃^– and Cl^-, and fulvic acid, however, the existence of SO₄^2- and CO₃^2– increased the degradation degree of CBZ. Toxicity tests were performed to determine the toxicity of untreated CBZ, and treated CBZ by photocatalytic, and sono-photocatalytic oxidations.     

Ultrasound with low intensity assisted the synthesis of nanocrystalline TiO2 without calcination

A novel method has been developed for the preparation of nano-sized TiO₂ with anatase phase. Nanoparticles with diameter about 6 nm were prepared at a relatively low temperature (75 °C) and short time. The synthesis was carried out by the hydrolysis of titanium tetra-isopropoxide (TTIP) in the presence of water, ethanol, and dispersant under ultrasonic irradiation (500 kHz) at low intensity. The results show that variables such as water/ethanol ratio, irradiation time, and temperature have a great influence on the particle size and crystalline phases of TiO₂ nanoparticles. Characterization of the product was carried out by different techniques such as powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and UV–vis spectroscopy.     

Ultrasonic-assisted synthesis of two dimensional coral-like Pd nanosheets supported on reduced graphene oxide for enhanced electrocatalytic performance

Two dimensional (2D) Pd nanosheets supported on reduced graphene oxide (Pd/rGO) were prepared through a sonochemical routine induced by cetyltrimethylammonium bromide (CTAB). Coral-like porous Pd nanosheets (Pd/rGO-u) were obtained under the sonication condition (25 kHz, 600 W, ultrasonic transducer), while square Pd nanosheets (Pd/rGO-c) were produced via traditional chemical reduction. The size of Pd nanosheets of Pd/rGO-u and Pd/rGO-c are 69.7 nm and 59.7 nm, and the thickness are 4.6 nm and 4.4 nm, respectively. The carrier GO was proved to be partially reduced to rGO with good electrical conductivity and oxygen-containing groups facilitated a good dispersion of Pd nanosheets. The interaction between GO and CTAB made the alkyl chain assembles to a 2D lamella micelles which limit the growth of Pd atoms resulting in the formation of 2D nanosheets. A high ultrasonic power promotes the reduction and the formation of porous structure. Additionally, Pd/rGO-u exhibited a favorable electrocatalytic performance toward oxygen reduction reaction (ORR) in alkaline condition, which provided a potential synthetic strategy assisted by sonication for high-performance 2D materials.     

Investigation of acoustic and geometric effects on the sonoreactor performance

In this work, three design configurations of a sonoreactor are considered under various operating conditions, and the acoustic characteristics during water sonication are investigated while using an immersed-type ultrasonic flat transducer probe in a sonoreactor model. Numerical models are also developed to simulate the sonication process, and they are successfully validated and compared with available data in the literature. Several sets of numerical investigations are conducted using the finite-element method and solved by the computational acoustics module in the COMSOL Multiphysics. The effects of the acoustical and geometrical parameters are investigated, analyzed, and reported, including the ultrasonic frequency, acoustic intensity, and scaling-up the reactor. The present study includes a parametric investigation examining the change of the ultrasonic frequency, intensity, and probe immersion depth on the performance. The results of the parametric study show that the highest cavitation energy corresponds to the maximum magnitude of negative pressure that takes place in the range of 60–80 kHz. The cavitation energy analyses are conducted under the conditions of 20 kHz of frequency and at 36 W input power. It is found that the cavitation energy of 15.87 W could produce 2.98 × 10⁻¹⁰ mol/J of sonochemical efficiency. In addition, the effect of altering the transducer probe depth changes the acoustic pressure field insignificantly. Furthermore, a recommendation is made to improve the sonochemical efficiency by introducing more considerable ultrasound input power while operating the sonoreactor at an ultrasonic frequency lower than 60 kHz. The results presented in this paper provide a comprehensive assessment of different sonoreactors and the feasibility of scaling-up their production rate.     

Ultrasound-assisted synthesis of ZnO photocatalysts for gas phase pollutant remediation: Role of the synthetic parameters and of promotion with WO3

The synthesis of ZnO photocatalysts by ultrasound-assisted technique was here investigated. Several experimental parameters including the zinc precursor (acetate, chloride, nitrate), sonication conditions (amplitude, pulse) and post-synthetic thermal treatment (up to 500 °C) were studied. Crystalline ZnO samples were obtained without thermal treatments due to the adopted reactant ratios and synthesis temperature. Sonication plays a major role on the morphological oxide features in terms of particle size and surface area, the latter showing a 20-fold increase with respect to conventional synthesis. Interestingly, 1 and 3 s sonication pulses led to morphological properties similar to continuous sonication. A thermal treatment at moderate temperatures (400–450 °C) promoted the loss of surface hydroxylation and the formation of lattice defects, while higher temperatures were detrimental for the sample morphology. The prepared ZnO was decorated with WO₃ particles comparing an ultrasound-assisted technique using 1 s pulses with a conventional approach, giving rise to composites with promoted visible light absorption. Samples were tested towards the photocatalytic degradation of nitrogen oxides (500–1000 ppb) in humidified air under both UV and visible light. By carefully controlling the synthetic procedure, better performance were observed with respect to the commercial benchmark. Samples from ultrasound-assisted syntheses, also in the case of pulsed sonication, showed consistently better results than conventional references, in particular for ZnO-WO₃ composites. The composite by ultrasound-assisted synthesis showed > 95% degradation in 180 min and doubled NO_x degradation under visible light with respect to the conventional composite.     

Tailoring the size of ultrasound responsive lipid-shelled nanodroplets by varying production parameters and environmental conditions

Liquid perfluorocarbon nanodroplets (NDs) are an attractive alternative to microbubbles (MBs) for ultrasound-mediated therapeutic and diagnostic applications. ND size and size distribution have a strong influence on their behaviour in vivo, including extravasation efficiency, circulation time, and response to ultrasound stimulation. Thus, it is desirable to identify ways to tailor the ND size and size distribution during manufacturing. In this study phospholipid-coated NDs, comprising a perfluoro-n-pentane (PFP) core stabilised by a DSPC/PEG40s (1,2-distearoyl-sn-glycero-3-phosphocholine and polyoxyethylene(40)stearate, 9:1 molar ratio) shell, were produced in phosphate-buffered saline (PBS) by sonication. The effect of the following production-related parameters on ND size was investigated: PFP concentration, power and duration of sonication, and incorporation of a lipophilic fluorescent dye. ND stability was also assessed at both 4 °C and 37 °C. When a sonication pulse of 6 s and 15% duty cycle was employed, increasing the volumetric concentration of PFP from 5% to 15% v/v in PBS resulted in an increase in ND diameter from 215.8 ± 16.8 nm to 408.9 ± 171.2 nm. An increase in the intensity of sonication from 48 to 72 W (with 10% PFP v/v in PBS) led to a decrease in ND size from 354.6 ± 127.2 nm to 315.0 ± 100.5 nm. Increasing the sonication time from 20 s to 40 s (using a pulsed sonication with 30% duty cycle) did not result in a significant change in ND size (in the range 278–314 nm); however, when it was increased to 60 s, the average ND diameter reduced to 249.7 ± 9.7 nm, which also presented a significantly lower standard deviation compared to the other experimental conditions investigated (i.e., 9.7 nm vs. > 49.4 nm). The addition of the fluorescent dye DiI at different molar ratios did not affect the ND size distribution. NDs were stable at 4 °C for up to 6 days and at 37 °C for up to 110 min; however, some evidence of ND-to-MB phase transition was observed after 40 min at 37 °C. Finally, phase transition of NDs into MBs was demonstrated using a tissue-mimicking flow phantom under therapeutic ultrasound exposure conditions (ultrasound frequency: 0.5 MHz, acoustic pressure: 2–4 MPa, and pulse repetition frequency: 100 Hz).     

Fabrication and characterization of quercetin loaded casein phosphopeptides-chitosan composite nanoparticles by ultrasound treatment: Factor optimization,formation mechanism,physicochemical stability and antioxidant activity

Ultrasound treatment was used to successfully prepare Quercetin (Qu)-loaded Casein phosphopeptides (CPP)/chitosan (CS) nanoparticles. Compared with the control, the above ternary nanoparticles with the smallest size (241.27 nm, decreased by 34.32%), improved encapsulation efficiency of Qu (78.55%, increased by 22.12%) when prepared under following conditions: ultrasonic frequency, 20/35/50 kHz; the power density, 80 W/L; the time, 20 min, and the intermittent ratio, 20 s/5s. Electrostatic interactions, hydrogen bonding, and hydrophobic interactions were the main driving forces for nanoparticles formulation, which were strengthened by ultrasound treatment. The compact, homogeneous and spherical composite nanoparticles obtained by sonication were clearly observed by scanning electron microscope and atomic force microscope. The environmental stability (NaCl, pH, exposure time, storage time, and simulated gastrointestinal digestion) and antioxidant activity of the ternary nanoparticles were remarkably enhanced after ultrasonic treatment. Furthermore, the ternary nanoparticles prepared by ultrasound exhibited excellent stability in simulated gastrointestinal digestion. The above results indicate that ultrasound not only increases the loading of the nanoparticles on bioactive substances but also improves the environmental stability and antioxidant activity of the formed nanoparticles. Ultrasound-assisted preparation of nanoparticles loaded with bioactive substances could be well used in the functional food and beverage industry.