Sonochemical synthesis of hydroxyapatite from H3PO4 solution with Ca(OH)2

Ultrasound was irradiated to an aqueous suspension containing phosphoric acid (H3PO4) and calcium hydroxide (Ca(OH)2) to investigate the sonochemical effect on preparation of hydroxyapatite (Ca10(PO4)6(OH)2, HAp). HAp monophase could be synthesized from the suspension sonicated for 60 min. The reaction for HAp was promoted more effectively than that of the heating method conducted at the same conditions as those for the sonicating method. The equilibrium pH of the suspensions sonicated over 60 min was maintained neutral, suggesting that the synthesis reaction was almost completed. The ultrasonic irradiation played an important role to progress the heterogeneous reaction and the preparation of very fine HAp powder.     

Wet chemical synthesis and characterization of pure and cerium doped Dy2O3 nanoparticles

Pure and cerium doped Dy₂O₃ nanoparticles were prepared by wet chemical synthesis route. The particles were subjected to thermal, structural, morphological and optical property studies. The calcination temperature was chosen based on the decomposition of the samples revealed by TG studies. EDS and FTIR results confirmed the presence of cerium in the Dy₂O₃ system. The particle size calculated from Williamson-Hall plot was consistent with TEM results. The effect of cerium as a dopant on the UV–vis absorption and photoluminescence intensity has been studied. XRD and PL analyses demonstrate that the cerium ions uniformly substitute dysprosium sites in Dy₂O₃ lattice and hence influence the optical properties.     

Sonochemical assisted synthesis of SrFe12O19 nanoparticles

We present the synthesis of M-type strontium hexaferrite by sonochemistry and annealing. The effects of the sonication time and thermal energy on the crystal structure and magnetic properties of the obtained powders are presented. Strontium hexagonal ferrite (SrFe₁₂O₁₉) was successfully prepared by the ultrasonic cavitation (sonochemistry) of a complexed polyol solution of metallic acetates and diethylene glycol. The obtained materials were subsequently annealed at temperatures from 300 to 900 °C. X-ray diffraction analysis shows that the sonochemical process yields an amorphous phase containing Fe³⁺, Fe²⁺ and Sr²⁺ ions. This amorphous phase transforms into an intermediate phase of maghemite (γ-Fe₂O₃) at 300 °C. At 500 °C, the intermediate species is converted to hematite (α-Fe₂O₃) by a topotactic transition. The final product of strontium hexaferrite (SrFe₁₂O₁₉) is generated at 800 °C. The obtained strontium hexaferrite shows a magnetization of 62.3 emu/g, which is consistent with pure hexaferrite obtained by other methods, and a coercivity of 6.25 kOe, which is higher than expected for this hexaferrite. The powder morphology is composed of aggregates of rounded particles with an average particle size of 60 nm.     

TDS and EELS observations for CO,O2, and CH3OH bound to Ru(0001)/Cu

The electronic properties of monolayers of copper atoms adsorbed onto a Ru(0001) single crystal surface have been studied with thermal desorption spectroscopy (TDS) and high resolution electron energy loss spectroscopy (EELS) utilizing carbon monoxide (CO), dioxygen (O₂), methanol (CH₃OH), and to some extent water (H₂O) as chemical probes. Whereas a three-monolayer-thick film exhibits most properties of a Cu(111) crystal distinct deviations are found at lower Cu coverages. TDS as well as EELS show a weakened RuCO bond and a strengthened CuCO bond as a result of metal-metal interaction. The stronger CuCO bond is accompanied by a higher probability for O₂ dissociation. The mobilities of copper and oxygen atoms are such that annealing to 650 K produces an overlayer structure which is independent of adsorption sequence: Cu/O₂ or O₂/Cu, but where RuO as well as CuO vibrations can be identified. Methanol adsorbs reversibly on a monolayer of copper atoms. Metal bound methoxy species are formed in the presence of oxygen atoms. The decomposition paths of such methoxy intermediates alter towards more formaldehyde (CH₂O) relative to CO with increasing copper and methoxy coverages.     

Selective synthesis of clinoatacamite Cu2(OH)3Cl and tenorite CuO nanoparticles by pH control

To investigate the shell deposited kinetics, CdSe quantum dots (QDs) and nanorods (NRs) with a maximum length of 17 nm were fabricated via organic synthesis routes. CdSe with a hexagonal crystal structure (wurtzite) favors epitaxial growth on the {002} surfaces when well-controlled conditions were used. The morphologies and sizes of CdSe samples depended strongly on chemicals and temperature. In the case of 320 °C, CdSe NRs with adjusted length of 7–17 nm were obtained from trioctylphosphine oxide (TOPO) and tetradecylphosphonic acid (TDPA). In contrast, short CdSe NRs (less than 10 nm) were created from octadecylphosphonic acid (ODPA) and trioctylamine (TOA). Spherical CdSe QDs were further fabricated using stearic acid (SA) and TOPO at 300 °C. CdSe cores were coated with Cd_0.5Zn_0.5S and CdTe shells. Anisotropic growth occurred during shell deposition because CdS shells grown preferentially on the {001} facet of the CdSe core. In the case of CdSe core prepared from TOPO and TDPA, CdSe/Cd_0.5Zn_0.5S core/shell samples prepared from long CdSe NRs (more than 10 nm) revealed a peanut morphology while the core/shell samples created from short ones (less than 10 nm) exhibited a spherical morphology. All of the CdSe/Cd_0.5Zn_0.5S core/shell samples revealed a similar length to that of the CdSe cores. This phenomenon was also observed for the core/shell samples fabricated using CdSe NRs prepared by ODPA and TOA. This is ascribed to the well-developed crystal structure of CdSe NRs fabricated using an organic synthesis at high temperature. In contrast, this anisotropic growth did not occur when spherical CdSe QDs prepared from SA and TOPO and the shell (Cd_0.5Zn_0.5S) coating carried out using SA and TOA. To indicate the shell depositing process, CdSe NRs fabricated using TDPA and TOPO were coated with a CdTe shell. CdTe monomers were deposited on the middle and tip parts of the CdSe NRs to form a tetrapod-like morphology at 220 °C. This is ascribed to the large difference of structure of CdSe (hexagonal) and CdTe (zinc blende).     

Sonochemical synthesis of TiO(2 nanoparticles on graphene for use as photocatalyst

Using ultrasonication we succeed in a controlled incorporation of TiO(2) nanoparticles on the graphene layers homogeneously in a few hours. The average size of the TiO(2) nanoparticles was controlled at around 4-5 nm on the sheets without using any surfactant, which is attributed to the pyrolysis and condensation of the dissolved TiCl(4) into TiO(2) by ultrasonic waves. The photocatalytic activity of the resultant graphene-TiO(2) composites containing 25 wt.% TiO(2) is better than that of commercial pure TiO(2). This is partly due to the extremely small size of the TiO(2) nanoparticles and partly due to the graphene-TiO(2) composite structure consisting of homogeneous dispersion of crystalline TiO(2) nanoparticles on the graphene sheets. As the graphene in the composites has a very good contact with the TiO(2) nanoparticles it enhances the photo-electron conversion of TiO(2) by reducing the recombination of photo-generated electron-hole pairs.     

Facile synthesis of hollow Fe2O3 nanotubes on nitrogen-doped graphene and their electrochemical performances

Ionics - The design and optimization of electrode materials are critically important for the development of high-performance supercapacitors. Herein, hollow Fe2O3 nanotubes supported on...     

Raman spectroscopy of dawsonite NaAl(CO3)(OH)2

Raman spectroscopy both at 298 and 77 K complemented with infrared spectroscopy was used to study the structure of dawsonite. Previous crystallographic studies concluded that the structure of dawsonite was a simple one; however, both Raman and infrared spectroscopy show that this conclusion is incorrect. Multiple bands are observed in both the Raman and infrared spectra in the antisymmetric stretching and bending regions, showing that the symmetry of the carbonate anion is reduced and in all probability the carbonate anions are not equivalent in the dawsonite structure. Multiple OH deformation vibrations centred around 950 cm⁻¹ in both Raman and infrared spectra show that the OH units in the dawsonite structure are non‐equivalent. Calculations using the position of the Raman and infrared OH stretching vibrations enabled estimates of the hydrogen‐bond distances of 0.2735 and 0.27219 pm at 298 K, and 0.27315 and 0.2713 pm at 77 K to be made. This indicates strong hydrogen bonding of the OH units in the dawsonite structure. Copyright © 2007 John Wiley & Sons, Ltd.     

Sonochemical preparation of composite nanoparticles of Au/gamma-Fe2O3 and magnetic separation of glutathione

We prepared Au/gamma-Fe2O3 composite nanoparticles by sonochemically reducing Au(III) ions employing no stabilizer in the aqueous solution to form stable Au nanoparticles and allowing them to attach onto the surface of gamma-Fe2O3 particles with an average size of 21 nm. Size of the formed Au nanoparticle depended on the initial concentration of Au(III) ions. The number of the Au nanoparticles, supported on each gamma-Fe2O3 particle was controlled by changing the relative amounts of Au(III) ions and gamma-Fe2O3 particles. The composite nanoparticles exhibited a high affinity with glutathione, a tripeptide with mercapto group so that separation and manipulation of glutathione in aqueous solutions could be performed by application of external magnetic field. Because the surfaces of the Au nanoparticles were not shielded by any stabilizers, or naked, sonochemically prepared Au/gamma-Fe2O3 composite nanoparticles seemed to show stronger affinity to the glutathione than those by the radiochemical method.     

Sonochemical synthesis and characterization of nano-sized lead(II) 3D coordination polymer: Precursor for the synthesis of lead(II) oxybromide nanoparticles

Nanoparticles of a three-dimensional coordination polymer, [Pb(L)(μ₂-Br)(H₂O)]_n (1), (L^? = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by an ultrasonic method and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal (DTA) analyses and compared each other. Concentration of initial reagents effects and the role of power ultrasound irradiation on size and morphology of nano-structured compound 1, have been studied. Calcination of the compound 1 at 500 °C under air atmosphere yields Pb₃O₂Br₂ nanoparticles.     

Eu-doped ZnO nanoparticles: Sonochemical synthesis,characterization, and sonocatalytic application

Undoped and europium (III)-doped ZnO nanoparticles were prepared by a sonochemical method. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS) analysis. The crystalline sizes of undoped and 3% Eu-doped ZnO were found to be 16.04 and 8.22 nm, respectively. The particle size of Eu-doped ZnO nanoparticles was much smaller than that of pure ZnO. The synthesized nanocatalysts were used for the sonocatalytic degradation of Acid Red 17. Among the Eu-doped ZnO catalysts, 3% Eu-doped ZnO nanoparticles showed the highest sonocatalytic activity. The effects of various parameters such as catalyst loading, initial dye concentration, pH, ultrasonic power, the effect of oxidizing agents, and the presence of anions were investigated. The produced intermediates of the sonocatalytic process were monitored by GC–Mass (GC–MS) spectrometry.     

Effect of the La(OH)3 preparation method on the surface and rehydroxylation properties of resulting La2O3 nanoparticles

In the present study, for the first time, Cu₃N/NiTiCu/Si heterostructures were successfully grown using magnetron sputtering technique. Nanocrystalline copper nitride (Cu₃N with thickness ~200 nm) thin films and copper nanodots were subsequently deposited on the surface of 2-μm-thick NiTiCu shape memory thin films in order to improve the surface corrosion and nickel release properties of NiTiCu thin films. Interestingly, the phase transformation from martensite phase to austenite phase has been observed in Cu₃N/NiTiCu heterostructures with corresponding change in texture and surface morphology of top Cu₃N films. Field emission scanning electron microscopy and atomic force microscope images of the heterostructures reveals the formation of 20-nm-sized copper nanodots on NiTiCu surface at higher deposition temperature (450 °C) of Cu₃N. Cu₃N passivated NiTiCu films possess low corrosion current density with higher corrosion potential and, therefore, better corrosion resistance as compared to pure NiTiCu films. The concentration of Ni released from the Cu₃N/NiTiCu samples was observed to be much less than that of pure NiTiCu film. It can be reduced to the factor of about one-ninth after the surface passivation resulting in smooth, homogeneous and highly corrosion resistant surface. The antibacterial and cytotoxicity of pure and Cu₃N coated NiTiCu thin films were investigated through green fluorescent protein expressing E. coli bacteria and human embryonic kidney cells. The results show the strong antibacterial property and non cytotoxicity of Cu₃N/NiTiCu heterostructure. This work is of immense technological importance due to variety of BioMEMS applications.     

Structural stability and conductivity of cubic (WO3)x - (Dy2O3)y-(Bi2O3)1−x−y

Isovalent rare earth oxide cubic stabilized bismuth oxides undergo an order-disorder transition of the oxygen sublattice ∼600 °C. Annealing below this temperature leads to a decay in conductivity due to ordering. We recently discovered a high conductivity Bi₂O₃ electrolyte doped with both Dy₂O₃ and WO₃ (DyWSB). The dopants were selected based on their polarizability and its effect on both structural stability and conductivity. Electrical conductivity results of the stabilized bismuth oxide system as function of temperature and time are presented. By manipulating the composition ratio of the dopants, the structural stability was enhanced resulting in a more stable conductivity.     

Sonochemical synthesis,formation mechanism,and solar cell application of tellurium nanoparticles

Tellurium inherently tends to form 1-D structures and while the 0-D Te nanostructures have better properties and applications in solar cell. In the present study, 0-D Te nanostructures including rice-like and spherical nanoparticles with the particle size of 15–40 nm were successfully synthesized via a facile sonochemical method. In the absence of ultrasonic irradiation nanorods were produced while performing the reaction under ultrasonic waves (at 200 W for 30 min) led to the formation of nanoparticles. Finally, the efficiency of various as-synthesized Te nanostructures in quantum dot-sensitized solar cells (QDSSCs) were evaluated. Using rice-like nanoparticles led to increase in J_SC, V_OC, FF and η parameters from 1.22, 0.54, 0.49 and 0.32% to 1.57, 0.64, 0.63 and 0.63%, respectively, compared with nanorods.     

Sonochemical synthesis, size controlling and gas sensing properties of NiO nanoparticles

Nanoparticles of NiO (NP-NiO) were prepared by a novel sonochemical route from Ni acetate and sodium hydroxide without any requirement of calcinations steps at high temperature and without surfactants. Drop casting of the nanocrystals onto alumina substrates allowed the fabrication of gas sensing devices, which were tested towards NO₂ and CO and showed promising results. At low working temperature, the NiO nanoparticles based sensors are selective to nitrogen oxide; in fact a good sensitivity is shown at 200 °C at low concentration (2 ppm), while at temperature above 350 °C, high responses are obtained for carbon monoxide. The results obtained are stimulating for further developing of NP-NiO based sensor devices.     

Sonochemical conversion of CO2 into hydrocarbons: The Sabatier reaction at ambient conditions

In this study, we investigated an alternative method for the chemical CO₂ reduction reaction in which power ultrasound (488 kHz ultrasonic plate transducer) was applied to CO₂-saturated (up to 3%) pure water, NaCl and synthetic seawater solutions. Under ultrasonic conditions, the converted CO₂ products were found to be mainly CH₄, C₂H₄ and C₂H₆ including large amount of CO which was subsequently converted into CH₄. We have found that introducing molecular H₂ plays a crucial role in the CO₂ conversion process and that increasing hydrogen concentration increased the yields of hydrocarbons. However, it was observed that at higher hydrogen concentrations, the overall conversion decreased since hydrogen, a diatomic gas, is known to decrease cavitational activity in liquids. It was also found that 1.0 M NaCl solutions saturated with 2% CO₂ + 98% H₂ led to maximum hydrocarbon yields (close to 5%) and increasing the salt concentrations further decreased the yield of hydrocarbons due to the combined physical and chemical effects of ultrasound. It was shown that CO₂ present in a synthetic industrial flue gas (86.74% N₂, 13% CO₂, 0.2% O₂ and 600 ppm of CO) could be converted into hydrocarbons through this method by diluting the flue gas with hydrogen. Moreover, it was observed that in addition to pure water, synthetic seawater can also be used as an ultrasonicating media for the sonochemical process where the presence of NaCl improves the yields of hydrocarbons by ca. 40%. We have also shown that by using low frequency high-power ultrasound in the absence of catalysts, it is possible to carry out the conversion process at ambient conditions i.e., at room temperature and pressure. We are postulating that each cavitation bubble formed during ultrasonication act as a “micro-reactor” where the so-called Sabatier reaction -$C{O}_2+4H_2\stackrel{\mathit{Ultrasonication}}{\to }C{H}_4+2H_{2}O$ - takes place upon collapse of the bubble. We are naming this novel approach as the “Islam-Pollet-Hihn process”.     

Synthesis and electrical properties of Y2O3: Dy3+ & Eu3+ nanoparticles

Yttrium oxide (Y₂O₃) doped with Dy³⁺ & Eu³⁺ nanoparticle has been synthesized by solution combustion method. The formation of the compounds has been checked by X-ray diffraction method. The crystallite/particle size has been measured using Scherrer formula as well as by transmission electron microscopy which show that the size of the particles are in the nanorange. The frequency and temperature dependent variation of impedance Z*, dielectric constant (ε′), dielectric loss (ε″) and AC conductivity (σ) of Y₂O₃: Dy³⁺ & Eu³⁺ nanoparticles were also measured. The real and imaginary part of complex impedance makes semicircle in the complex plane. The center of semicircle arc is found to be shifted toward higher value of real part of impedance with increasing temperature. This indicates that the conductivity of the material increases with the increase in temperature. Cole–Cole plots demonstrate that the dielectric relaxation process occurs in the material. The AC conductivity (σ _AC) increases with the increase in temperature within the frequency range of 10³–10⁷ Hz confirming the hopping of the electrons in the conduction process. The value of impedance decreases sharply with increasing frequency and attains minimum value after 10⁵ Hz at all temperatures.     

Sonochemical synthesis of Cu2O nanocubes for enhanced chemiluminescence applications

A facile one-step sonochemical synthesis of Cu₂O nanocubes has been developed by ultrasound irradiation of copper sulfate in the presence of polyvinylpyrrolidone and ascorbic acid at pH 11. During sonication, the reaction between acoustic cavitation-generated radicals and CuSO₄ produced Cu(OH)₂ intermediate which then reacted with ascorbic acid to generate Cu₂O nanocubes. The products were characterized by FT-IR, XRD, HRTEM, AFM and particle size analyzer. The prepared Cu₂O nanocubes were found to be very effective for enhancing chemiluminescence in the presence of luminol–H₂O₂ system.