Electrochemical synthesis of Ag nanoparticles supported on glassy carbon electrode by means of p-isopropyl calix[6]arene matrix and its application for electrocatalytic reduction of H2O2

The silver nanoparticles were prepared on the glassy carbon (GC) electrode, modified with p-iso propyl calix[6]arene, by preconcentration of silver ions in open circuit potential and followed by electrochemical reduction of silver ions. The stepwise fabrication process of Ag nanoparticles was characterized by scanning electron microscopy and electrochemical impedance spectroscopy. The prepared Ag nanoparticles were deposited with an average size of 70 nm and a homogeneous distribution on the surface of electrode. The observed results indicated that the presence of calixarene layer on the electrode surface can control the particle size and prevent the agglomeratione and electrochemical deposition is a promising technique for preparation of nanoparticles due to its easy-to-use procedure and low cost of implementation. Cyclic voltammetry experiments showed that Ag nanoparticles had a good catalytic ability for the reduction of hydrogen peroxide (H₂O₂). The effects of p-isopropyl calix[6]arene concentration, applied potential for reduction of Ag⁺, number of calixarene layers and pH value on the electrocatalytic ability of Ag nanoparticles were investigated. The present modified electrode exhibited a linear range from 5.0 × 10⁻⁵ to 6.5 × 10⁻³ M and a detection limit 2.7 × 10⁻⁵ M of H₂O₂ (S/N = 3) using amperometric method.     

rf reactive co-sputtered Au-Ag alloy nanoparticles in SiO2 thin films

We have studied formation of Au-Ag alloy nanoparticles in sputtered SiO₂ thin films. Silica thin films containing Au-Ag nanoparticles were deposited on quartz substrates using rf reactive magnetron co-sputtering technique. The films heat-treated in reducing Ar + H₂ atmosphere at different temperatures. They were analyzed by using UV-vis spectrophotometry, atomic force microscopy and X-ray photoelectron spectroscopy (XPS) methods for their optical, surface morphological as well as structural and chemical properties. The optical absorption of the Au-Ag alloy nanoparticles illustrated one plasmon resonance absorption peak located at 450 nm between the absorption bands of pure Au and Ag nanoparticles at 400 and 520 nm, respectively, for the thin films annealed at 800 °C. XPS results showed that the alloys were in metallic state, and they had a greater tendency to lose electrons as compared to their corresponding monometallic state. Using lateral force microscopy analysis, we have found that the alloy particles were uniformly distributed on the surface with grain size of about 20 nm.     

Optical properties of surface-modified Bi2O3 nanoparticles

Stearic acid coated Bi₂O₃ nanoparticles in the size range of 5-13 nm were synthesized by the microemulsion method. HRTEM showed that the morphology of Bi₂O₃ nanoparticles was ellipsoidal. The absorption edge of Bi₂O₃ nanoparticles showed a blue shift of ∼0.45 eV, comparing with that of the bulk Bi₂O₃. At room temperature, Bi₂O₃ nanoparticles also showed a strong luminescence at 397 and 420 nm, depending on the excitation wavelength.     

Functionalization of lamellar molybdenum disulphide nanocomposite with gold nanoparticles

This work explores the functionalization of an organic-inorganic MoS₂ lamellar compound, prepared by a chemical liquid deposition method (CLD), that has an interlamellar distance of ∼5.2 nm, using clusters of gold nanoparticles. The gold nanoparticles have a mean diameter of 1.2 nm, a stability of ∼85 days, and a zeta potential measured to be ζ = −6.8 mV (solid). The nanoparticles are localized in the hydrophilic zones, defined by the presence of amine groups of the surfactant between the lamella of MoS₂. SEM, TEM, EDAX and electron diffraction provide conclusive evidence of the interlamellar insertion of the gold nanoparticles in the MoS₂.     

High-density plasma etching of indium-zinc oxide films in Ar/Cl2 and Ar/CH4/H2 chemistries

The dry etching characteristics of transparent and conductive indium-zinc oxide (IZO) films have been investigated using an inductively coupled high-density plasma. While the Cl₂-based plasma mixture showed little enhancement over physical sputtering in a pure argon atmosphere, the CH₄/H₂/Ar chemistry produced an increase of the IZO etch rate. On the other hand, the surface morphology of IZO films after etching in Ar and Ar/Cl₂ discharges is smooth, whereas that after etching in CH₄/H₂/Ar presents particle-like features resulting from the preferential desorption of In- and O-containing products. Etching in CH₄/H₂/Ar also produces formation of a Zn-rich surface layer, whose thickness (∼40 nm) is well-above the expected range of incident ions in the material (∼1 nm). Such alteration of the IZO layer after etching in CH₄/H₂/Ar plasmas is expected to have a significant impact on the transparent electrode properties in optoelectronic device fabrication.     

Dielectric behavior of nano-structured and bulk Li Ni Zn ferrite samples

The ac conductivity and dielectric properties of spinel ferrite nanoparticles of Li_0.1(Ni_1−xZn_x)_0.8Fe_2.1O₄ (x=0.0–1.0) prepared by the chemical co-precipitation method were investigated as functions of frequency and temperature by using a complex impedance technique. Parts of the precipitated powders were pressed into a disk-shape and were sintered at 1473 K for 2 h to increase the particle size to the bulk scale (dimensions >100 nm). The ac conductivity of the samples increases with increasing temperature, ensuring the semiconducting behavior of both nano and bulk samples, in agreement with the Koops model to describe heterogeneous structures. The significant decrease in ac conductivity σ′_ac, dielectric constant, and dielectric loss of the as-prepared nanosamples compared to their bulk counterparts is correlated to the small size of the grain compared to the grain boundary size. This might be useful for many applications requiring the reduction of eddy current effects.     

Exchange bias in Co nanoparticles embedded in an Mn matrix

Magnetic properties of Co nanoparticles of 1.8 nm diameter embedded in Mn and Ag matrices have been studied as a function of the volume fraction (VFF). While the Co nanoparticles in the Ag matrix show superparamagnetic behavior with T_B=9.5 K (1.5% VFF) and T_B=18.5 K (8.9% VFF), the Co nanoparticles in the antiferromagnetic Mn matrix show a transition peak at ∼65 K in the ZFC/FC susceptibility measurements, and an increase of the coercive fields at low temperature with respect to the Ag matrix. Exchange bias due to the interface exchange coupling between Co particles and the antiferromagnetic Mn matrix has also been studied. The exchange bias field (H_eb), observed for all Co/Mn samples below 40 K, decreases with decreasing volume fraction and with increasing temperature and depends on the field of cooling (H_fc). Exchange bias is accompanied by an increase of coercivity.     

A novel approach for the synthesis of superparamagnetic Mn3O4 nanocrystals by ultrasonic bath

In this study, the synthesis of Mn₃O₄ (husmannite) nanoparticles was carried out in two different alkali media under sonication by ultrasonic bath and conventional method. Manganese acetate was used as precursor, sodium hydroxide and hexamethylenetetramine (HMT) as basic reagents in this synthesis. An ultrasonic bath with low intensity was used for the preparation of nanomaterials. The as prepared samples were characterized with X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (HRTEM, TEM), energy-dispersive spectrum (EDS), and superconducting quantum interference device (SQUID) analysis. The XRD patterns exhibit the nanocrystals are in pure tetragonal phase. The chemical composition was obtained by EDS analysis and confirmed the presence of Mn and O in the sample. According to the TEM and HRTEM results, both nanorods and nanoparticles of Mn₃O₄ were obtained in the presence of ultrasonic irradiation. The average size of nanoparticles was 10 nm, and the size of nanorods was 12 nm in diameter and 100-900 nm in length for the samples prepared in basic medium with sodium hydroxide. In the conventional method with the same basic medium, the nanorod was not observed and the nearly cubic nanoparticles was appeared with an average size of 2.5 nm. The selected area electron diffraction (SAED) patterns revealed that the nanocrystals are polycrystalline in nature. When HMT was used as a basic reagent in the presence of ultrasonic irradiation, it was led to a higher size of nanoparticles and nanorods than when sodium hydroxide was used as a basic reagent. The average size of nanoparticles was about 15 nm and its shape was nearly cubic. The diameter for nanorods was 50 nm and the length was about a few micrometers.The magnetic measurements were carried out on the sample prepared in sodium hydroxide under ultrasonic irradiation. These measurements as a function of temperature and field strength showed a reduction in ferrimagnetic temperature (T_c = 40 K) as compared to those reported for the bulk (T_c = 43 K). The superparamagnetic behavior was observed at room temperature with no saturation magnetization and hysteresis in the region of measured field strength.     

Synthesis and magnetic characterization of nickel ferrite nanoparticles prepared by co-precipitation route

Magnetic nanoparticles of nickel ferrite (NiFe₂O₄) have been synthesized by co-precipitation route using stable ferric and nickel salts with sodium hydroxide as the precipitating agent and oleic acid as the surfactant. X-ray diffraction (XRD) and transmission electron microscope (TEM) analyses confirmed the formation of single-phase nickel ferrite nanoparticles in the range 8-28 nm depending upon the annealing temperature of the samples during the synthesis. The size of the particles (d) was observed to be increasing linearly with annealing temperature of the sample while the coercivity with particle size goes through a maximum, peaking at ∼11 nm and then decreases for larger particles. Typical blocking effects were observed below ∼225 K for all the prepared samples. The superparamagnetic blocking temperature (T_B) was found to be increasing with increasing particle size that has been attributed to the increased effective anisotropy energy of the nanoparticles. The saturation moment of all the samples was found much below the bulk value of nickel ferrite that has been attributed to the disordered surface spins or dead/inert layer in these nanoparticles.     

Magnetorheology of colloidal dispersion containing Fe nanoparticles synthesized by the arc-plasma method

Spherical crystalline Fe nanoparticles, ∼100 nm in diameter, were synthesized under Ar-50% H₂ arc-plasma. These nanoparticles were dispersed in silicone oil after silane treatment on as-grown thin oxide layer (∼2 nm) to make their surfaces hydrophobic. The resulting Fe nanoparticles exhibited a high saturation magnetization of ∼190 emu/g at room temperature. The static magnetorheological behavior was measured for the colloidal dispersion (solid concentration: 15 vol%) at room temperature under magnetic flux densities of 0-0.3 T, using a parallel-plate-type commercial rheometer. The yield stress continuously increased with magnetic flux density, demonstrating the Bingham plastic behavior. Moreover, subjecting the sample to a magnetic flux density of 0.3 T increased the yield stress by ∼10². Additionally, the colloidal dispersion exhibited good stability against sedimentation.     

Evolution of surface morphology of NiO thin films under swift heavy ion irradiation

NiO nanoparticle thin films grown on Si substrates were irradiated by 107 MeV Ag⁸⁺ ions. The films were characterized by glancing angle X-ray diffraction and atomic force microscopy. Ag ion irradiation was found to influence the shape and size of the nanoparticles. The pristine NiO film consisted of uniform size (∼100 nm along major axis and ∼55 nm along minor axis) elliptical particles, which changed to also of uniform size (∼63 nm) circular shape particles on irradiation at a fluence of 3 × 10¹³ ions cm⁻². Comparison of XRD line width analysis and AFM data revealed that the particles in the pristine films are single crystalline, which turn to polycrystalline on irradiation with 107 MeV Ag ions.     

1064-nm laser fragmentation of thin Au and Ag flakes in acetone for highly productive pathway to stable metal nanoparticles

The laser-induced fragmentation of thin Au and Ag flakes in acetone by 1064-nm nanosecond laser (with the fluence typically ∼2 J/cm²) potentially offers a highly productive pathway to stable metal nanoparticles in liquid. Acetone serves as a superior liquid medium that keeps fine metal nanoparticles free from precipitation even in such concentrated nanoparticle solutions exceeding ∼0.1 M. Thin metal flakes have good capability to absorb the 1064-nm laser energy as efficiently as in the visible region. A part of the thus laser-heated molten flakes explosively split into submicroparticles, and some other significant part directly into fine nanoparticles. Both kinds of product particles have minor absorption cross-sections for subsequent laser pulses at 1064 nm, and thus no longer fragment further. One of the two kinds of Ag flakes studied in this work yielded fine Ag nanoparticles at a remarkable high production rate of 1.1 mg/min for the input laser power of only ∼0.65 W.     

Formation of gold nanoparticles in heat-treated reactive co-sputtered Au-SiO2 thin films

In this work, formation of gold nanoparticles in radio frequency (RF) reactive magnetron co-sputtered Au-SiO₂ thin films post annealed at different temperatures in Ar + H₂ atmosphere has been investigated. Optical, surface topography, chemical state and crystalline properties of the prepared films were analyzed by using UV-visible spectrophotometry, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD) techniques, respectively. Optical absorption spectrum of the Au-SiO₂ thin films annealed at 800 °C showed one surface plasmon resonance (SPR) absorption peak located at 520 nm relating to gold nanoparticles. According to XPS analysis, it was found that the gold nanoparticles had a tendency to accumulate on surface of the heat-treated films in the metallic state. AFM images showed that the nanoparticles were uniformly distributed on the film surface with grain size of about 30 nm. Using XRD analysis average crystalline size of the Au particles was estimated to about 20 nm.     

Effect of H2 and O2 plasma etching treatment on the surface of diamond-like carbon thin film

In this study, we investigated the surface properties of diamond-like carbon (DLC) films for biomedical applications through plasma etching treatment using oxygen (O₂) and hydrogen (H₂) gas. The synthesis and post-plasma etching treatment of DLC films were carried out by 13.56 MHz RF plasma enhanced chemical vapor deposition (PECVD) system. In order to characterize the surface of DLC films, they were etched to a thickness of approximately 100 nm and were compared with an as-deposited DLC film. We obtained the optimum condition through power variation, at which the etching rate by H₂ and O₂ was 30 and 80 nm/min, respectively. The structural and chemical properties of these thin films after the plasma etching treatment were evaluated by Raman and Fourier transform infrared (FT-IR) spectroscopy. In the case of as-deposited and H₂ plasma etching-treated DLC film, the contact angle was 86.4° and 83.7°, respectively, whereas it was reduced to 35.5° in the etching-treated DLC film in O₂ plasma. The surface roughness of plasma etching-treated DLC with H₂ or O₂ was maintained smooth at 0.1 nm. These results indicated that the surface of the etching-treated DLC film in O₂ plasma was hydrophilic as well as smooth.     

Synthesis and characterization of nanostructured Ag on porous titania

In this work, porous titania was prepared on bulk Ti by chemical oxidation, and then nanostructured silver (Ag) was deposited on titania surface by ion beam sputtering. After annealing treatment, Ag/TiO₂ composites were characterized using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Results indicated that a nano-porous titania layer with mean pore size of 150 nm and thickness of 1 μm was formed by chemical oxidation at 80 °C for 45 min. There were three Ag species (Ag (0), Ag (1+), and Ag (2+)) on composites surface after annealing treatment, and metallic Ag content achieved maximum value with annealing temperature of 500 °C in air. Ag showed high thermal stability being partly attributed to the inhibiting the diffusion of Ag by the underlying porous titania.     

Green chemistry-mediated synthesis of nanostructures of afterglow phosphor

Various nanostructures of SrAl₂O₄:Eu²⁺, Dy³⁺ (SAC) afterglow phosphor were prepared in a single-step reaction using a green chemistry-mediated modified combustion process. The evolution of hazardous NxOx gases during the customary combustion reaction was completely eliminated by employing an innovative complex formation route. Another fascinating feature of the process was that, a slight change in the processing conditions ensured the synthesis of either nanoparticles or nanowires. The photoluminescence spectrum of nanophosphor showed a slight blue shift in emission (∼511 nm) as compared to the bulk phosphor (∼520 nm). The afterglow (decay) profiles of SAC nanoparticles, nanowires and bulk phosphor were compared. The chemistry underlying the nanostructure synthesis and the probable afterglow mechanism were discussed.     

On 308 nm photofragmentation of the silver nanoparticles

Silver nanoparticles (Ag NPs) were prepared by different chemical methods possessing different sizes 3 ± 2, 8 ± 2, and 20 ± 5 nm. The influence the size of Ag NPs was demonstrated by the absorption and fluorescence spectra, the maximum absorption of Ag NPs increases as the particle size increases. When Ag NPs irradiated with 308 nm excimer laser; the maximum absorption and the full width at half maximum decreased as the number of pulses increased up to 100,000 pulse; due to the size reduction. The fluorescence spectra of Ag NPs and irradiated Ag NPs with 308 nm excimer laser were recorded after excitation at 441.5 nm He-Cd laser, showing a red shift increasing as the particle size is increased.     

Effect of Co underlayer on soft magnetic properties and microstructure of FeCo thin films

High saturation magnetization soft magnetic FeCo (=Fe₆₅Co₃₅) films were prepared using a thin Co underlayer. The FeCo/Co films exhibited a well-defined in-plane uniaxial anisotropy with easy axis coercivity (H_ce) of 10 Oe and hard axis coercivity (H_ch) of 3 Oe, and a half reduction of H_c with H_ce=4.8 Oe and H_ch=1.0 Oe was obtained when the composition was adjusted to 25 at% Co. The effective permeability of the films remains flat around 250 to 800 MHz. The saturation magnetostriction was 5.2×10⁻⁵ and the intrinsic stress was 0.8 GPa in FeCo single layer, both were slightly reduced by Co underlayer. The Co underlayer changed the preferred orientation of the FeCo films from (2 0 0) to (1 1 0) but more significantly, reduced the average grain size from ∼74 to ∼8.2 nm. It also reduced the surface roughness from 2.351 to 0.751 nm. The initial stage and interface diffusion properties were examined by TEM and XPS.     

Non-linear optical properties of silver nanoparticles prepared by hydrogen reduction method

Silver nanoparticles have been prepared using hydrogen gas as the reducing agent for silver nitrate and poly(vinyl pyrrolidone) as the capping agent; the reaction was carried out at 70 °C for 3 h. The size of the nanoparticles was found to be about 20 nm as analyzed using transmission electron micrographs. The X-ray diffraction pattern revealed the face-centered cubic (fcc) structure of silver nanoparticles. The linear absorption of Ag nanoparticles, α, is obtained about 3.71 cm⁻¹. The non-linear refractive indices of silver nanoparticles were defined by the z-scan technique using CW He-Ne laser (λ = 632.8 nm) at different incident intensities. The magnitude of non-linear refractive index (n₂) was measured to be in the order of 10⁻⁷ (cm²/W) with a negative sign. Therefore self-defocusing phenomena is taking placed for Ag nanoparticles.     

Synthesis and magnetic characterization of Zn0.6Ni0.4Fe2O4 nanoparticles via a polyethylene glycol-assisted hydrothermal route

Zn-doped nickel ferrite nanoparticles (Zn_0.6Ni_0.4Fe₂O₄) have been prepared via a surfactant, polyethylene glycol assisted hydrothermal route. X-ray powder diffractometry (XRD), Fourier transform infrared spectroscopy, transmission electron microscopy (TEM), and vibrating scanning magnetometry (VSM) were used for the structural, morphological, and magnetic characterizations of the product, respectively. TEM analysis revealed that the nanoparticles have a narrow size distribution, with average particle size of 15±1 nm, which agrees well with the XRD based estimate of 14±2 nm. The absence of saturation and remanent magnetization, and coercivity in the high temperature region of the M-H curve and non-zero magnetic moments indicate superparamagnetism of the nanoparticles with a canted spin structure. The appearance of a peak on the temperature-dependent zero-field cooling magnetization curve at ∼190 K indicates the blocking temperature of the sample.