Intensification of extraction of curcumin from Curcuma amada using ultrasound assisted approach: Effect of different operating parameters

Curcumin, a dietary phytochemical, has been extracted from rhizomes of Curcuma amada using ultrasound assisted extraction (UAE) and the results compared with the conventional extraction approach to establish the process intensification benefits. The effect of operating parameters such as type of solvent, extraction time, extraction temperature, solid to solvent ratio, particle size and ultrasonic power on the extraction yield have been investigated in details for the approach UAE. The maximum extraction yield as 72% was obtained in 1 h under optimized conditions of 35 °C temperature, solid to solvent ratio of 1:25, particle size of 0.09 mm, ultrasonic power of 250 W and ultrasound frequency of 22 kHz with ethanol as the solvent. The obtained yield was significantly higher as compared to the batch extraction where only about 62% yield was achieved in 8 h of treatment. Peleg’s model was used to describe the kinetics of UAE and the model showed a good agreement with the experimental results. Overall, ultrasound has been established to be a green process for extraction of curcumin with benefits of reduction in time as compared to batch extraction and the operating temperature as compared to Soxhlet extraction.     

Intensification of alkaline delignification of sugarcane bagasse using ultrasound assisted approach

Ultrasound-assisted approach has been investigated for delignification so as to develop green and sustainable technology. Combination of NaOH with ultrasound has been applied with detailed study into effect of various parameters such as time (operating range of 15–90 min), alkali concentration (0.25 M−2.5 M), solvent loading (1:15–1:30 w/v), temperature (50–90 ˚C), power (40–140 W) and duty cycle (40–70 %) at fixed frequency of 20 kHz. The optimized operating conditions established for the ultrasonic horn were 1 M as the NaOH concentration, 1 h as treatment time, 70˚C as the operating temperature, 1:20 as the biomass loading ratio, 100 W as the ultrasonic power and 70% duty cycle yielding 67.30% as the delignification extent. Comparative study performed using conventional and ultrasonic bath assisted alkaline treatment revealed lower delignification as 48.09% and 61.55% respectively. The biomass samples were characterized by SEM, XRD, FTIR and BET techniques to establish the role of ultrasound during the treatment. The morphological changes based on the ultrasound treatment demonstrated by SEM were favorable for enhanced delignification and also the crystallinity index was more in the case of ultrasound treated material than that obtained by conventional method. Specific surface area and pore size determinations based on BET analysis also confirmed beneficial role of ultrasound. The overall results clearly demonstrated the intensification obtained due to the use of ultrasonic reactors.     

Intensification of paracetamol (acetaminophen) synthesis from hydroquinone using ultrasound

Paracetamol (acetaminophen) is one of the most frequently used analgesic and antipyretic drugs. This work deals with ultrasound assisted synthesis (UAS) of paracetamol from hydroquinone using ammonium acetate as an amidating agent. The optimization of various reaction and ultrasound parameters was performed to minimize the energy and time requirement. UAS of paracetamol was achieved at a lower temperature (60 °C) and the time (150 min) without formation of salt as a byproduct, making reaction green and inherently safer. On the other hand, the conventional process requires high reaction temperature (220 °C) and time (15 h). The quantification of the product was done by using high performance liquid chromatography (HPLC). Optimization of parameters revealed that the percent yield of 57.72% can be obtained in 150 min by performing the reaction in the ultrasound bath at 22 kHz frequency, 60 °C temperature, hydroquinone to ammonium acetate and acetic acid in a molar ratio of 1:6:5, 125 W power, 50% duty cycle and agitation speed of 300 RPM. Hence, ultrasound assisted synthesis can be considered as a process intensification tool for the synthesis of paracetamol and possibly other pharmaceutical compounds.     

Process intensification of synthesis of metal organic framework particles assisted by ultrasound irradiation

This study synthesized UiO-66, a typical Zr-Metal Organic Framework (MOF), by using an ultrasound-assisted synthesis method to reduce the synthesis time. This method was short-time ultrasound irradiation at the initial stage of the reaction. As compared with average particle size of conventional solvothermal method (=192 nm), averaged particle size by the ultrasound-assisted synthesis method showed particle sizes that were smaller on average, ranging from 56 to 155 nm. In order to compare the relative reaction rates of the solvothermal method and the ultrasound-assisted synthesis method, the cloudiness of the reaction solution in the reactor was observed with a video camera, and the luminance was calculated from the images obtained by the video camera. It was found that the ultrasound-assisted synthesis method showed a faster increase in luminance and shorter induction time than the solvothermal method. The slope of the luminance increase during the transient period was also found to become increase with the addition of ultrasound, which also affects the growth of particles. Observation of the aliquoted reaction solution confirmed that particle growth was faster in the ultrasound-assisted synthesis method than in the solvothermal method. Numerical simulations were also performed using MATLAB ver. 5.5 to analyze the unique reaction field generated by ultrasound. Bubble radius and temperature inside a cavitation bubble was obtained using the Keller-Miksis equation, which reproduces the motion of a single bubble. The bubble radius expanded and contracted repeatedly according to the ultrasound sound pressure, and eventually collapsed. The temperature at the time of collapse was extremely high, exceeding 17,000 K. It was confirmed that the high-temperature reaction field generated by ultrasound irradiation promoted nucleation, leading to a reduction in particle size and induction time.     

Intensification of dilute acid hydrolysis of spent tea powder using ultrasound for enhanced production of reducing sugars

Spent tea (ST) powder is one of the potential sustainable sources available abundantly and can be utilized to produce reducing sugars required for production of platform chemicals. The current study aims at intensifying the reducing sugars production based on ultrasound assisted dilute acid hydrolysis (UADAH). The effects of reaction time, solid liquid ratio, acid concentration and temperature on the yield of reducing sugars were investigated initially for UADAH process based on ultrasonic (US) horn. The highest yield of 24.75 g/L for the reducing sugars was obtained at solid liquid ratio of 1:8, acid concentration of 1% w/v and temperature of 60 °C within 120 min. Use of oxidants like hydrogen peroxide (H₂O₂) and Fenton’s reagent to further intensify the production has also been studied. Use of H₂O₂ at optimum loading of 0.75 g/L resulted in reducing sugars yield of 26.2 g/L within 75 min while using same H₂O₂ loading with FeSO₄ at loading of 0.75 g/L along with UADAH reduced the reaction time to 60 min for almost similar yield. Large scale studies performed using US flow cell revealed that yield of reducing sugars as 22.4 g/L is obtained in 120 min in the case of only UADAH, while in the case of UADAH along with H₂O₂ and Fenton’s reagent, similar yield of reducing sugars was obtained in only 90 and 60 min respectively. UADAH in combination with oxidants has been demonstrated as an effective and intensified approach to produce reducing sugars from spent tea powder available as sustainable source.     

Synergistic effects of negative-charged nanoparticles assisted by ultrasound on the reversal multidrug resistance phenotype in breast cancer cells

We have fabricated a negative-charged nanoparticle (Heparin-Folate-Tat-Taxol NP, H-F-Tat-T NP) with dual ligands, tumor targeting ligand folate and cell-penetrating peptide Tat, to deliver taxol presenting great anticancer activity for sensitive cancer cells, while it fails to overcome multidrug resistance (MDR) in MCF-7/T cells (taxol-resistant breast cancer cells). Ultrasound (US) can increase the sensitivity of positive-charged NPs thereby making it possible to reverse MDR through inducing NPs’ drug release. However, compared with the negative-charged NPs, positive-charged NPs may cause higher toxic effect. Hence, the combination of negative-charged NPs and US may be an efficient strategy for overcoming MDR. The conventional procedure to treat with NPs followed by US exposure possibly destruct multifunctional NPs resulting in its bioactivity inhibition. Herein, we have further improved the operating approach to eliminate US mechanical damage and keep the integrity of negative-charged NPs: cells are exposed to US with microbubbles (MBs) prior to the treatment of H-F-Tat-T NPs. Superior to the conventional method, US sonoporation affects the physiological property of cancer cells while preventing direct promotion of drug release from NPs. The results of the present study displayed that US in condition (1 MHz, 10% duty cycle, duration of 80 s, US intensity of 0.6 W/cm² and volume ratio of medium to MBs 20:1) combined with H-F-T-Tat-T NPs can achieve optimal reversal MDR effect in MCF-7/T cells. Mechanism study further disclosed that the individual effect of US was responsible for the enhancement of cell membrane permeability, inhibition of cell proliferation rate and down-regulation of MDR-related genes and proteins. Simultaneously, US sonoporation on resistant cancer cells indirectly increased the accumulation of NPs by inducing endosomal escape of negative-charged NPs. Taken together, the overcoming MDR ability for the combined strategy was achieved by the synergistic effect from individual function of NPs, physiological changes of resistant cancer cells and behavior changes of NPs caused by US.     

Ultrasound assisted acid catalyzed lactose hydrolysis: Understanding into effect of operating parameters and scale up studies

The current work deals with the value addition of lactose by transforming into hydrolyzed lactose syrup containing glucose and galactose in major proportion using the novel approach of ultrasound assisted acid catalyzed lactose hydrolysis. The hydrolysis of lactose was performed in ultrasonic bath (33 kHz) at 50% duty cycle at different temperatures as 65 °C and 70 °C and two different hydrochloric acid (HCl) concentrations as 2.5 N and 3 N. It was observed that acid concentration, temperature and ultrasonic treatment were the major factors in deciding the time required to achieve ∼90% hydrolysis. The ultrasonic assisted approach resulted in reduction in the reaction time and the extent of intensification was established to be dependent on the temperature, acid concentration and time of ultrasonic exposure. It was observed that the maximum process intensification obtained by introduction of ultrasound in the lactose hydrolysis process performed at 70 °C and 3 N HCl was reduction in the required time for ∼90% hydrolysis from 4 h (without the presence of ultrasound) to 3 h. The scale-up study was also performed using an ultrasonic bath with longitudinal horn (36 kHz as operating frequency) at 50% duty cycle, optimized temperature of 70 °C and acid concentration of 3 N. It was observed that the reaction was faster in the presence of ultrasound and stirring by axial impeller at rpm of 225 ± 25. The time required to complete ∼90% of hydrolysis remained almost the same as observed for small scale study on ultrasonic bath (33 kHz) at 50% duty cycle. The use of recovered lactose from whey samples instead of pure lactose did not result in any significant changes in the progress of hydrolysis, confirming the efficacy of the selected approach. Overall, the work has presented a novel ultrasound assisted approach for intensified lactose hydrolysis.     

Intensification of heterogeneously catalyzed Suzuki-Miyaura cross-coupling reaction using ultrasound: Understanding effect of operating parameters

Palladium-catalyzed Suzuki-Miyaura cross-coupling reaction is a significant reaction for obtaining industrially important products. The current research work deals with intensification of reaction of 4-bromoanisole and phenylboronic acid catalyzed with 5 wt% Pd/C (5% by weight Pd supported on C available as commercial catalyst) using ultrasound and more importantly, without use of any additional phase transfer catalyst. Heterogeneous catalyst has been selected in the present work so as to harness the benefits of easy separation and the possible limitations of heterogeneous operation are minimized by introducing ultrasonic irradiations. The effect of operating parameters such as ultrasound power, temperature, catalyst loading and molar ratio on the progress of reaction has been investigated. It has been observed that an optimum power, temperature and catalyst loading exist for maximum benefits whereas higher molar ratio was found to be favourable for the progress of the reaction. Also, the use of ultrasound reduced the reaction time from 70 min required in conventional approach to only 35 min under conditions of frequency of 22 kHz, power dissipation of 40 W and catalyst loading as 1.5 mol% (refers to total quantum of catalyst used in the work) in ethanol-water system under ambient conditions. The work also demonstrated successful results at ten times higher volume as compared to the normally used volumes in the case of simple ultrasonic horn. Overall, the work has successfully demonstrated process intensification benefits obtained due to the use of ultrasound for heterogeneously catalyzed Suzuki-Miyaura cross-coupling reaction.     

Tracer studies of anodic films formed on aluminium in malonic and oxalic acids

Using a tungsten-containing layer, incorporated into sputtering-deposited aluminium, as a tracer, the growth of porous anodic films in malonic and oxalic acid electrolytes has been investigated using transmission electron microscopy, Rutherford backscattering spectroscopy and nuclear reaction analysis. Comparisons were also made with films formed in phosphoric acid electrolyte, which have been studied previously. The findings reveal a distortion of the tracer layer within the barrier region of the porous films, evident as a lagging of the tracer beneath the pores relative to that in the adjacent cell wall region. Further, the films are significantly thicker than the layer of metal consumed during anodizing and display smooth-sided pores. The anodizing behaviours are consistent with a major role for field-assisted flow of film material within the barrier layer in the development of the pores.     

Triple-combination therapy assisted with ultrasound-active gold nanoparticles and ultrasound therapy against 3D cisplatin-resistant ovarian cancer model

Cancer chemotherapy suffers from drug resistance and side effects of the drugs. Combination therapies have been attracted attention to overcome these limitations of traditional cancer treatments. Recently, increasing in intracellular chemotherapeutic concentration in the presence of ultrasonic waves (US) has been shown in the preclinical stage. In addition, some recent studies have shown that nanoparticles increase the effectiveness of ultrasound therapy. In this study, the US-active property of gold nanocones (AuNCs) was utilized for combinational US and cisplatin (Cis) to overcome drug resistance. The effect of the triple combination therapy US + AuNCs + Cis with low-dose Cis on 2/3D models of cisplatin-resistant ovarian cancer cell line (A2780cis) were investigated. In the 2D cell culture, 60% of the A2780cis cell population was suppressed with triple combination therapy; and the long-term therapeutic efficacy of the US + AuNCs + Cis with the low-dose drug was demonstrated by suppressing 83% of colony formation. According to the results in the 3D cell model, 60% of the spheroid formation was suppressed by the triple combination therapy with low-dose Cis. These results not only demonstrate the success of the US + AuNCs + Cis triple combination therapy for its long-term therapeutic effect on resistant cancer cells but also verified that it might enable effective cancer therapy in vivo and clinical stages based on the 3D tumor models. In addition, enhanced anti-cancer activity was demonstrated at the low-dose Cis on drug-resistant cancer cells indicating the triple-combination therapy successfully overcame drug resistance and this is a promising strategy to reduce the side effects of chemotherapy. This work exhibits a novel US and AuNCs-mediated combination cancer therapy, which demonstrates the role of ultrasound-active AuNCs to combat drug resistance with low-dose chemotherapy.     

Improving effect of oleic acid-mediated sodium caseinate-based encapsulation in an ultrasound field on the thermal stability and bioaccessibility of quercetin

The simultaneous improvement of quercetin (QUE) processing stability and bioavailability has always presented a technical challenge during food processing. This study constructed a water-soluble carrier consisting of oleic acid (OA) and sodium caseinate (NaCas) in an ultrasonic field and investigated the effect of its encapsulation on improving the thermal stability and bioaccessibility of QUE. The results showed that the OA and NaCas generated uniform, stable water-soluble particles with a poly dispersity index (PDI) below 0.3 and an absolute value of Zeta potential above 30 mV in optimized conditions (a protein concentration of 4 mg/mL, ultrasonic power of 300 W, and ultrasonic time of 5 min). OA-NaCas mass ratio of 1:40, 1:15, 1:8, and 1:4 was selected for QUE loading to compare its encapsulation effect at different mass ratios. Compared with the NaCas without OA, the QUE embedding rate reached 95 % at OA-NaCas mass ratios of 1:15 and 1:8. In addition, the transmission electron microscopy (TEM) images confirmed that QUE was embedded in OA-NaCas particles, forming regular, spherical OA-NaCas-QUE particles at mass ratios or 1:15 and 1:8. Next, when heated at 80 °C for 120 min, the OA-NaCas (OA:NaCas, 1:15, 1:8, and W/W) particles significantly improved the QUE retention rate. The simulated in vitro gastrointestinal digestion experiments showed that the QUE bioaccessibility increased from 25 % to more than 60 % when it was encapsulated in OA-NaCas (OA:NaCas, 1:15, 1:8, and W/W) particles. These results indicated that the OA-NaCas complex was suitable as a hydrophilic delivery carrier of fat-soluble polyphenols.     

Investigate the ultrasound energy assisted adsorption mechanism of nickel(II) ions onto modified magnetic cobalt ferrite nanoparticles: Multivariate optimization

In present study, magnetic cobalt ferrite nanoparticles modified with (E)-N-(2-nitrobenzylidene)-2-(2-(2-nitrophenyl)imidazolidine-1-yl) ethaneamine (CoFe₂O₄-NPs-NBNPIEA) was synthesized and applied as novel adsorbent for ultrasound energy assisted adsorption of nickel(II) ions (Ni²⁺) from aqueous solution. The prepared adsorbent characterized by Fourier transforms infrared spectroscopy (FT-IR), transmission electron microscope (TEM), vibrating sample magnetometer (VSM) and X-ray diffraction (XRD). The dependency of adsorption percentage to variables such as pH, initial Ni²⁺ ions concentration, adsorbent mass and ultrasound time were studied with response surface methodology (RSM) by considering the desirable functions. The quadratic model between the dependent and independent variables was built. The proposed method showed good agreement between the experimental data and predictive value, and it has been successfully employed to adsorption of Ni²⁺ ions from aqueous solution. Subsequently, the experimental equilibrium data at different concentration of Ni²⁺ ions and 10 mg amount of adsorbent mass was fitted to conventional isotherm models like Langmuir, Freundlich, Tempkin, Dubinin-Radushkevich and it was revealed that the Langmuir is best model for explanation of behavior of experimental data. In addition, conventional kinetic models such as pseudo-first and second-order, Elovich and intraparticle diffusion were applied and it was seen that pseudo-second-order equation is suitable to fit the experimental data.     

Controllable manipulation of crystallinity and morphology of aluminium surfaces using high intensity ultrasound

High intensity ultrasound (HIUS) provides highly non-equilibrium condition for metal processing. Controllable manipulation of crystallinity and morphology of metal coatings is important for different applications including catalysis and corrosion protection. Investigation of effects of HIUS in different sonication media on microstructure and morphology of aluminium (Al) layers showed that HIUS can cause melting and recrystallization of Al. Due to high cooling rate the grain size of Al can be reduced. Ultrasonically induced structure refinement could potentially be used for enhancement of mechanical properties of coatings. If ultrasonically generated temperature is not high enough for metal melting, temperature induced atomic diffusion leads to grain growth, segregation and fragmentation of Al layers and, thus, the formation of attractive for catalytic application increased surface area.     

Ultrasonic cavitation: An effective cleaner and greener intensification technology in the extraction and surface modification of nanocellulose

With rising consumer demand for natural products, a greener and cleaner technology, i.e., ultrasound-assisted extraction, has received immense attention given its effective and rapid isolation for nanocellulose compared to conventional methods. Nevertheless, the application of ultrasound on a commercial scale is limited due to the challenges associated with process optimization, high energy requirement, difficulty in equipment design and process scale-up, safety and regulatory issues. This review aims to narrow the research gap by placing the current research activities into perspectives and highlighting the diversified applications, significant roles, and potentials of ultrasound to ease future developments. In recent years, enhancements have been reported with ultrasound assistance, including a reduction in extraction duration, minimization of the reliance on harmful chemicals, and, most importantly, improved yield and properties of nanocellulose. An extensive review of the strengths and weaknesses of ultrasound-assisted treatments has also been considered. Essentially, the cavitation phenomena enhance the extraction efficiency through an increased mass transfer rate between the substrate and solvent due to the implosion of microbubbles. Optimization of process parameters such as ultrasonic intensity, duration, and frequency have indicated their significance for improved efficiency.     

Sonochemical approach for synthesis of zinc oxide-poly methyl methacrylate hybrid nanoparticles and its application in corrosion inhibition

Hybrid nanoparticles (HNPs) with zinc oxide and polymethyl metha acrylate (inorganic/ polymer) were synthesized through the exploitation of ultrasound approach. The synthesized HNPs were further characterized employing transmission electron microscopy and x-ray diffraction. ZnO-PMMA based HNPs exhibit excellent protection properties to mild steel from corrosion when gets exposed to acidic condition. Electrochemical impendence spectroscopy (EIS) analysis was accomplished to evaluate the corrosion inhibition performance of MS panel coated with 2 wt% or 4 wt% of HNPs and its comparison with bare panel and that of loaded with only standard epoxy coating., Tafel plot and Nyquist plot analysis depicted that the corrosion current density (I_corr) decreases from 16.7 A/m² for bare material to 0.103 A/m² for 4% coating of HNPs. Applied potential (E_corr) values shifted from negative to positive side. These results were further supported by qualitative analysis. The images taken over a period of time indicated the increase in lifetime of MS panel from 2 to 3 days for bare panel to 10 days for HNPs coated panel, showing that ZnO-PMMA HNPs have potential application in metal protection from corrosion by forming a passive layer.     

Intensification of depolymerization of polyacrylic acid solution using different approaches based on ultrasound and solar irradiation with intensification studies

Depolymerization of polyacrylic acid (PAA) as sodium salt has been investigated using ultrasonic and solar irradiations with process intensification studies based on combination with hydrogen peroxide (H₂O₂) and ozone (O₃). Effect of solar intensity, ozone flow and ultrasonic power dissipation on the extent of viscosity reduction has been investigated for individual treatment approaches. The combined approaches such as US + solar, solar + O₃, solar + H₂O₂, US + H₂O₂ and US + O₃ have been subsequently investigated under optimum conditions and established to be more efficient as compared to individual approaches. Approach based on US (60 W) + solar + H₂O₂ (0.01%) resulted in the maximum extent of viscosity reduction as 98.97% in 35 min whereas operation of solar + H₂O₂ (0.01%), US (60 W), H₂O₂ (0.3%) and solar irradiation resulted in about 98.08%, 90.13%, 8.91% and 90.77% intrinsic viscosity reduction in 60 min respectively. Approach of US (60 W) + solar + ozone (400 mg/h flow rate) resulted in extent of viscosity reduction as 99.47% in 35 min whereas only ozone (400 mg/h flow rate), ozone (400 mg/h flow rate) + US (60 W) and ozone (400 mg/h flow rate) + solar resulted in 69.04%, 98.97% and 98.51% reduction in 60 min, 55 min and 55 min respectively. The chemical identity of the treated polymer using combined approaches was also characterized using FTIR (Fourier transform infrared) spectra and it was established that no significant structural changes were obtained during the treatment. Overall, it can be said that the combination technique based on US and solar irradiations in the presence of hydrogen peroxide is the best approach for the depolymerization of PAA solution.     

Subsurface deformation studies of aluminium during wear and its theoretical understanding using molecular dynamics

Adopting the bonded interface technique for wear experiments under vacuum, this paper reports the nature of the localised shear bands that appear at the different deformation zones of the subsurface of aluminium under different sliding conditions. The plastic deformations are mapped under both low load/low sliding velocities as well as high load and high sliding velocities. A monotonic change in local plastic strain as a function of depth at low sliding velocities give way to a discontinuity separating two different zones with differing plastic behaviour for high sliding speed wear test. Besides shear bands, bonded interface also reveals the presence of kinks particularly in the samples subjected to wear test with high sliding velocities. A molecular dynamic simulation of the wear process successfully replicated the experimental observation, thus allowing us to discuss the mechanism of subsurface deformation during the wear process in the absence of any significant oxide layer for aluminium under sliding condition.     

A facile one-pot ultrasound assisted for an efficient synthesis of benzo[g]chromenes using Fe3O4/polyethylene glycol (PEG) core/shell nanoparticles

In this research, a general synthetic method for the synthesis of benzo[g]chromenes has been developed using Fe₃O₄/polyethylene glycol (PEG) core/shell nanoparticle under ultrasonic irradiations. Compared to the conventional methods, ultrasound procedure showed several advantages including mild reaction conditions, high yield products, short reaction times, reusability of the catalyst and little catalyst loading.     

Synthetic antibacterial agent assisted synthesis of gold nanoparticles: Characterization and application studies

In this study, we report synthesis of water-soluble gold nanoparticles (Au-NPs), having an average diameter of ca. ∼20 nm, using ciprofloxacin (CF) as a reducing/stabilizing agent. The synthesized Au-NPs have been characterized by scanning electron microscopy (SEM), EDX, TEM, UV-visible spectroscopy (UV-vis), X-ray diffraction and cyclic voltammetry. TEM and SEM combined with EDX analysis confirmed that spherical-shaped Au-NPs were formed. UV-vis spectra of the Au-NPs showed two absorption bands corresponding to the capping agent ciprofloxacin and surface plasmon absorption bands at 274 and 527 nm, respectively. The synthesized Au-NPs are used to modify a glassy carbon electrode (GCE) and its electrochemical and electrocatalytic properties are investigated. The Au-NPs modified electrode showed excellent electrocatalytic activity towards the oxidation of methanol at +0.33 V in alkaline solution, which was not observed on the unmodified GCE. Further, electrocatalytic reduction of oxygen was also studied using the Au-NPs modified electrode at lower potential. Here, CF was used as a reducing agent for the preparation of Au-NPs dispersion. This Au-NPs dispersion is highly stable, and can be stored for more than three months in air at room temperature.     

Biomimetic nucleation and growth of hydrophobic vaterite nanoparticles with oleic acid in a methanol solution

Hydrophobic vaterite nanoparticles were prepared via crystallization of CaCO₃ with oleic acid in methanol by mimicking the process of biomineralization. The molar ratio of oleic acid to calcium ion was varied from 0.1 to 0.5. By changing the concentration of the oleic acid, CaCO₃ particles with different shapes and polymorphism were obtained. High concentration of the oleic acid gave stable vaterite crystals, the polymorph of which did not change when the composite was kept in water for more than one week. Fourier transform infrared spectroscopy (FT-IR) and TGA analysis of the obtained product indicated that the oleic acid was bound to the crystalline CaCO₃. The contact angle of the modified vaterite reached 122°. We have succeeded in crystallization of hydrophobic CaCO₃ nanoparticles in situ.