Extending LaMer's mechanism using open system for increasing forced and controlled growth of Au nano particles: Desired decreasing Fe3O4 nano particles size during simultaneous synthesis in optimized conditions

The most effective parameters were found to obtain Au/Fe₃O₄ nano particles (NPs)-oleylamine composite. Having Au NPs with the controlled maximum mean size under the forced conditions was the main aim of this study. We used the continuous flow rates of oleylamine 75% to produce Au NPs under an open system by extended LaMer mechanisms. This process decreased the mean size of Fe₃O₄ NPs synthesized simultaneously, by classic LaMer mechanism. The Fe₃O₄ NPs production was carried out without continuous adding of any iron reactant, viz. as a closed system. In the absence of gold ions, the mean size of the synthesized Fe₃O₄ NPs using 2.5 ml/min oleylamine was about 35.0 nm at 2.0 ± 0.5 °C after 120 min. This mean size was decreased to 27.2, 21.4, 16.8 and 8.7 nm, when Au NPs were simultaneous prepared using 0.5, 0.75, 1.5 and 2.5 ml/min of oleylamine, respectively, at the same conditions. Surface Plasmon Resonance (SPR) adsorption was used to evaluate Au NPs production at first 30 min, while Small Angle X-ray Scattering (SAXS) method was used to monitor the reaction progression for near-real time analysis of increasing the growth of Au NPs up to 280 min, at the optimum conditions. Changing the properties of Fe₃O₄ NPs during processes was determined by studying Magnetization, Potentiometric titration, Inductive heating and Zeta potential.     

Synthesis and magnetic properties of shuriken-like nickel nanoparticles

Shuriken-like nickel nanoparticles were successfully synthesized by a thermal decomposition method at 200 °C with Nickel(II) acetylacetonate (Ni(acac)₂) as the precursor and oleylamine (OAm) as the solvent and reductant, respectively. The phase structures, morphologies and sizes, and magnetic properties of the as-synthesized nickel products were characterized in detail by using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM). Some key reaction parameters, such as the reaction time, reaction temperature and surfactants, have important influence on the morphology of the final products. XRD pattern indicated that the products are well-crystallized face-centered cubic (fcc) nickel phase. SEM images demonstrated that the nickel nanoparticles are shuriken-like morphology with average size around 150 nm. The mechanism of shuriken-like Ni nanoparticles (NPs) is proposed. The magnetic hysteresis loops of shuriken-like and spherical nickel products illustrated the ferromagnetic nature at 300 K, indicating its potential applications in magnetic storage.     

The effect of molybdenum on optical properties of ZnO nanoparticles in Ultraviolet–Visible region

Zn_1?xMo_xO (x = 0.0, 0.01, 0.03, and 0.05) nanoparticles (NPs) are synthesized by using gelatin, via the sol-gel method. A calcination temperature of 600 °C is maintained for 2 h. The influence of molybdenum concentration on the structural and optical properties of these NPs is demonstrated. Synthesized NPs are characterized using X-ray diffraction (XRD), UV–vis spectroscopy, and transmission electron microscopy (TEM). XRD patterns reveal the crystallite nature of samples that exist in the hexagonal wurtzite phase. TEM images manifest the existence of nearly spherically-shaped NPs. The UV–vis spectroscopy results showed that the absorption edge of ZnO nanoparticles is red-shifted by adding molybdenum. Finally, the optical parameters of the refractive index and permittivity of the synthesized samples were calculated using Kramers-Kronig relations using the UV–vis spectra.     

Na0.5Li0.5CoO2 nanopowders: Facile synthesis,characterization and their application for the removal of methylene blue dye from aqueous solution

In this paper, delafossite-type Na_0.5Li_0.5CoO₂ nanoparticles (NPs) with an average particle size of 50 nm were successfully synthesized by sol–gel method. Prepared NPs were characterized by differential thermal analysis, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and scanning tunneling microscopy. The nanoparticles showed the excellent adsorption properties towards methylene blue dye (MBD) as a reactive dye. The kinetics of removal of MBD in aqueous solutions was studied in a series of experiments which were varied in the amount of NPs, contact time, pH, and temperature. The experimental data were fitted very well in the pseudo-second order kinetic model and the Freundlich adsorption isotherm model. 92% of dye was successfully removed in 10 min using 0.02 g Na_0.5Li_0.5CoO₂ NPs in a pH = 11. Thermodynamic study indicates that the adsorption of MBD is feasible, and spontaneous in nature.     

Highly dispersible and uniform size Cu2ZnSnS4 nanoparticles for photocatalytic application

Highly dispersible, uniform size (～7 nm) single-phase Cu₂ZnSnS₄ nanoparticles have been synthesized by hydrothermal method using non-toxic surfactant (oleic acid). High resolution transmission electron microscopy image indicates good crystallinity of the Cu₂ZnSnS₄ nanoparticles with the growth along (1 1 2) plane. X-ray photoelectron spectroscopy analyses suggested that the formation of with Cu, Zn, and Sn in +1, +2 and +4 oxidation states. The optical absorption spectrum of Cu₂ZnSnS₄ nanoparticles exhibits an absorption in the visible region and its optical band gap was found to be ～1.72 eV, which could be much more appropriate for photocatalytic application under visible light irradiation. These Cu₂ZnSnS₄ nanoparticles have been shown high photocatalytic degradation activity of methylene blue (MB) dye in the presence of visible light irradiation. The rate constant (k) value of Cu₂ZnSnS₄ nanoparticles is found to be 0.0144 min^?1. We have discussed the mechanism of dye degradation process that drives the photocatalytic degradation process. The reusability of the Cu₂ZnSnS₄ nanoparticles for the dye degradation is also demonstrated.     

Synthesis and characterization of novel magnetically separable NiFe2O4@AlMCM-41-Cu2O core-shell and its performance in removal of dye

The synthesis of magnetic NiFe₂O₄@AlMCM-41-Cu₂O core-shell as a new class of visible light driven photocatalyst was suggested. The magnetic NiFe₂O₄ core was prepared by solvothermal method. The intermediate AlMCM-41 shell was prepared by the method of liquid crystal templating mechanism and subsequently cuprous oxide (Cu₂O) nanoparticles (NPs) were synthesized in NiFe₂O₄@AlMCM-41core-shell via colloidal chemistry approach. The properties of prepared magnetic core-shell were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), nitrogen adsorption–desorption measurement and vibration sample magnetometer (VSM). Based on EDX results, the weight percentage (wt%) of NiFe₂O₄ core, MCM-41 shell and Cu₂O NPs were calculated to be 68.89, 30.55 and 0.56%, respectively. It consisted of mesoporous structure with a surface area of 687.00 m² g^?1, an average pore size of 2.95 nm and possessed excellent magnetic properties of 4.74 emu g^?1. The TEM results indicated that the NiFe₂O₄ as core were regular spheres with diameter of 68 nm, and the average thickness of AlMCM-41 shells was ～35 nm. The particles size of Cu₂O incorporated in core-shell was less than 5 nm. The photocatalytic activity was evaluated under visible light irradiation using the removal of methylene blue (MB) dye as a model reaction. The removal rate of MB achieved up to 90% after 60 min under visible light irradiation, and the NiFe₂O₄@AlMCM-41-Cu₂O can be recycled and reused.     

Vitis vinifera peel polyphenols stabilized gold nanoparticles induce cytotoxicity and apoptotic cell death in A431 skin cancer cell lines

Gold nanoparticles (AuNPs) are considered beneficial in the field of biomedicine and in the development of therapeutic nanomedicine products. In the present study, Vitis vinifera. L (grapes) peel polyphenols were utilized as reducing and stabilizing agents for the biosynthesis of gold nanoparticles, and their cytotoxicity and apoptotic effects were assessed. The synthesized gold nanoparticles were characterized using UV-Visible spectroscopy, Transmission electron microscopy (TEM), X-ray diffraction (XRD), Particle size distribution, Fourier transform infrared spectroscopy (FTIR) and zeta potential analysis. TEM analysis confirmed that the nanoparticles were spherical with ～20–40 nm in size. Particle size distribution revealed ～50 ± 5 nm nanoparticles and FTIR confirmed the presence of polyphenols capped onto the peel gold nanoparticles. The V. vinifera peel gold nanoparticles were studied for their antiproliferative activities and induction of apoptosis at the inhibitory concentration (IC₅₀) of 23.6 µM. A431 cell lines incubated with V. vinifera peel gold nanoparticles for 24 h exhibited cytotoxicity activity mediated by increased reactive oxygen species (ROS) production, apoptotic morphological changes and loss of membrane potential significantly (p < 0.01). Thus, the cytotoxicity of the gold nanoparticles could be attributed to the synergistic effects of the phenolic moieties of the V. vinifera peels and the efficiency of the bioconjugated gold nanoparticles causing apoptosis and secondary necrosis.     

Novel synthesis of hafnium oxide nanoparticles by precipitation method and its characterization

Hafnium oxide nanoparticles (HfO₂ NPs) have been successfully synthesized by means of a novel precipitation method and were characterized by using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Field emission scanning electron microscopy (FESEM), UV–visible, Fourier transform infrared (FTIR) and laser Raman spectroscopy. The XRD and Raman analysis revealed the presence of pure monoclinic HfO₂ NPs. FESEM image showed that the HfO₂ NPs were of spherical shape with an average particle size of about 20 nm. The optical band gap of the HfO₂ NPs was found to be 6.12 eV. Advantages of this method were simple and low cost of synthesis of HfO₂ NPs includes the small and narrow particle size distribution.     

Physical and optical properties of HfO2 NPs – Synthesis and characterization in finding its feasibility in opto-electronic devices

HfO₂ nanoparticles (HfO₂ NPs) with different precursors (NaOH, H₂O, ethanol) were synthesized by a simple co-precipitation method. FTIR and EDX spectroscopy analysis shows the Stoichiometries composition of HfO₂ NPs. X-ray diffraction pattern analysis revealed that the as prepared and calcined HfO₂ NPs are respectively amorphous and polycrystalline nature. TEM analysis confirms that the morphology of the calcined HfO₂ NPs is spherical in shape with less agglomeration. The crystallite size was evaluated to be 51 nm, 37 nm and 30 nm respectively, for the precursors NaOH, H₂O and ethanol used for HfO₂ NPs. SEM analysis shows spherical, rock and sponge like surface morphology respectively, for the precursors NaOH, H₂O and ethanol used for HfO₂ NPs. UV–visible spectroscopy analysis revealed that the optical band gap energy of NaOH, H₂O and ethanol precursors used HfO₂ NPs were respectively 5.50 eV, 5.52 eV and 5.50 eV. The observed optical properties indicated the feasibility of utilizing these NPs as anti reflection layers in solar cells and for the construction of poultry farms to save energy. The estimated dielectric constant value indicated that these NPs could be used to prepare dielectric layers in thin film transistor.     

Synthesis and photoluminescence of Ca1-xTiO3:xEu3+ nanoparticles

Ca_1-xTiO₃:xEu³⁺ nanoparticles (NPs) with the size ranging from 27 nm to 135 nm were prepared by means of a chemical co-precipitation method. The structural and optical properties of the NPs were investigated, and the influence of Eu doping content and sintering temperature on the photoluminescence of the Ca_1-xTiO₃:xEu³⁺ NPs were examined. An obvious red emission band centered at 615 nm were observed under the excitation with 395 nm for the Ca_1-xTiO₃:xEu³⁺ NPs. X-ray photoelectron spectroscopy analyses suggest that Eu³⁺ is incorporated into not only the Ca-site, but also Ti-site of CaTiO₃ crystal lattice. Our study shows the promise of the Ca_1-xTiO₃:xEu³⁺ NPs as a red nanophosphor.     

Amorphization and nanocrystalline Nb3Al intermetallic formation during mechanical alloying and subsequent annealing

In this paper the formation as well as the stability of Nb₃Al intermetallic compounds from pure Nb and Al metallic powders through mechanical alloying (MA) and subsequent annealing were studied. According to this method, the mixture of powders with the proportion of Nb-25 at% Al were milled under an argon gas atmosphere in a high-energy planetary ball mill, at 7, 14, 27 and 41 h, to fabricate disordered nanocrystalline Nb₃Al. The solid solution phase transitions of MA powders before and after annealing were characterized using X-ray diffractometry (XRD). The microstructural analysis was performed using scanning electron microscopy (SEM) as well as transmission electron microscopy (TEM). The results show that in the early stages of milling, Nb(Al) solid solution was formed with a nanocrystalline structure that is transformed into the amorphous structure by further milling times. Amorphization would appear if the milling time was as long as 27 h. Partially ordered Nb₃Al intermetallic could be synthesized by annealing treatment at 850 °C for 7 h at lower milling times. The size of the crystallites after subsequent annealing was kept around 45 nm.     

Structural,electrical, and rheological properties of palladium/silver bimetallic nanoparticles prepared by conventional and ultrasonic-assisted reduction methods

Polyvinylpyrrolidone stabilized Pd/Ag bimetallic nanoparticles (NPs) with average particle sizes of 9 and 6 nm were synthesized by simultaneous reduction in the presence and absence of ultrasound waves, respectively. The prepared NPs were characterized by six methods including X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution-TEM (HRTEM), UV–vis spectroscopy, scanning tunneling microscopy (STM), and energy dispersive X-ray (EDX) analysis. The rheological properties of Pd/Ag NPs in ethylene glycol as a base fluid with various mass fractions of NPs from 2% to 5% at different temperatures were studied experimentally and theoretically. The experimental results showed that viscosity of Pd/Ag NPs in ethylene glycol increases with increasing particle mass fraction and decreases with increasing temperature. A maximum of 31.58% increase in viscosity of ethylene glycol at 20 °C was observed when 5% Pd/Ag NPs was added. Measurement of the electrical conductivity of nanofluids of Pd/Ag bimetallic NPs in distilled water at different mass fractions and temperatures was performed. A 3841% increase in electrical conductivity of distilled water at 25 °C was observed when 1% Pd/Ag NPs was added. Both the rheological and electrical properties of Pd/Ag bimetallic NPs were measured in ethylene glycol and distilled water, respectively for the first time.     

Bio-directed synthesis of gold nanoparticles using Ananas comosus aqueous leaf extract and their photocatalytic activity for LDPE degradation

A bio-directed synthesis of gold nanoparticles (Au NPs) was developed via the reduction of hydrogen tetrachloroaurate (III) (HAuCl₄·3H₂O) solution by the aqueous leaf extract of Ananas comosus. The polyphenol stabilized Au NPs were characterized by UV–visible, Fourier transform infrared (FTIR), powder X-ray diffraction (PXRD)/selected area electron diffraction (SAED), high resolution transmission electron microscopy (HRTEM) and energy-dispersive X-ray spectroscopy (EDX) analyses. The HRTEM images revealed that Au NPs were well dispersed with spherical structures. The size ranges from 7.39 to 32.09 nm with average particle size of 18.85 ± 6.74 nm. The peaks of XRD analysis at (2θ) 37.96°, 44.06°, 64.54°, 77.50° and 81.73° were respectively assigned to (1 1 1), (2 0 0), (2 2 0), (3 1 1) and (2 2 2) planes of the face-centered cubic (fcc) lattice of gold. The photocatalytic potential of Au NPs was studied through the solid-phase degradation of low-density polyethylene (LDPE) film. The photoinduced degradation of LDPE@Au nanocomposite film was higher than that of the pure LDPE film. The weight loss of LDPE@Au (1.0 wt%) nanocomposite film steadily increased and reached 51.4 ± 4.8% in 240 h under solar light irradiation, compared to the photo-induced LDPE with only 8.6 ± 0.7%. However, LDPE film with 1.0% Au NPs gave a weight loss value of 4.72 ± 0.71 under the dark condition at the end of 240 h. Thus, LDPE film with 1.0% Au NPs showed a degradation efficiency of 90.8% under solar irradiation after 240 h. The sustainability of the nanoparticles was confirmed through reusability in the photocatalytic degradation reaction up to five consecutive cycles without substantial loss in its catalytic performance.     

Fabrication of Ag nanoparticles dispersed in PVA nanowire mats by microwave irradiation and electro-spinning

In this study, the antimicrobial substance, silver nanoparticles (Ag NPs) loaded in poly (vinyl alcohol) (PVA) nanowire mats were fabricated by conjugation of the electro-spinning method and the microwave-assisted process. The best PVA nanowire mats were fabricated by through control of electro-spinning conditions, which were applied for fabrication of Ag NPs loaded in PVA nanowires. PVA was used not only as a carrier for loading of Ag NPs but also as a reduction agent with which the Ag⁺ ion was already reduced to a large number of Ag NPs by irradiation with a microwave. Ag NPs were synthesized inside the PVA solution depending on the time of microwave irradiation — whether for 60 s or 90 s. Size distribution of Ag NPs was 5–10 nm in diameter for 60 s; and 10–20 nm in diameter for 90 s of irradiation. Presence of Ag NPs acquired through microwave assisted irradiation was confirmed by X-ray diffraction profiles (XRD). Microstructure, particle size distribution, and morphology of both the nanowire mats and the Ag particles were investigated using SEM and TEM techniques. The effect of Ag-NPs on the PVA mechanical property of nano-fibrous mats was investigated according to tensile strength. Antibacterial activity of PVA loaded Ag NPs at different irradiation times was tested on Gram-positive bacteria, Staphylococcus aureus Gram-negative bacteria, and Escherichia coli.     

Microbial synthesis of semiconductor lead sulfide nanoparticles using immobilized Rhodobacter sphaeroides

A reliable and eco-friendly process for the synthesis of nanoparticles such as using biological systems has been developed. In this study, we synthesized PbS nanoparticles with the average particle size ca. 10.5 ± 0.15 nm using immobilized Rhodobacter sphaeroides. The PbS nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive analyses of X-rays (EDX) and Uv–vis optical absorption. Culture time, as an important physiological parameter for R. sphaeroides growth, could significantly control the size of the biosynthesized lead sulfide nanoparticles. Extracellular synthesis of nanoparticles by immobilized mass could be highly advantageous from the point of view of synthesis in large quantities and easy downstream processing.     

Synthesis of hydroxysodalite zeolite by alkali-activation of basalt powder rich in calc-plagioclase

Hydroxysodalite (H-SOD) microcrystalline particles were synthesized from basalt powder rich in calcic-plagioclase (anorthite) by alkali activation at 80 °C/24 h. Sodium hydroxide (NaOH) solution was used as alkaline activator. The reactivity of the natural solid precursor basalt was studied using differential scanning calorimetry (DSC), and a maximum reaction enthalpy of (?ΔH) of 170 J/g was obtained. The chemical, mineralogical, and textural properties were obtained by using X-ray powder diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and N₂-adsorption-desorption measurements. The synthesized material has a specific BET surface area of 20.5 m² g^?1 approximately 200 times higher than raw basalt material (0.1 m² g^?1). The compressive strength of basalt based H-SOD/sand composite samples cured at 80 °C for 24 h upon using different amounts of the activator (NaOH) was evaluated under dry and saturated conditions. The dry samples with NaOH/basalt mass ratio of 0.12 have reached a compressive strength of 57 MPa. Wet samples, on the other hand, showed a compressive strength of 25 MPa after seven days of soaking in water and four episodes of wetting and drying. The present work illustrates that crystalline H-SOD could be synthesized from cheap basalt powder precursor.     

A 12R long-period stacking-ordered structure in a Mg-Ni-Y alloy

A hitherto unreported long-period stacking-ordered (LPSO) phase, designated 12R, was observed in a Mg₈₀Ni₅Y₁₅ (at.%) alloy. Microstructure was investigated by electron diffraction and high-angle annular dark-field scanning transmission electron microscopy. Results show that the 12R has a trigonal lattice (a = b = 1.112 nm, c = 3.126 nm, α = β = 90°, and γ = 120°). Unit cell of the 12R is consisted of three ABCA-type building blocks and each building block contains dominant Ni₆Y₈-type building clusters. A sound structural model is proposed based on relative positions of Ni₆Y₈ clusters in neighboring building blocks.     

A novel green synthesis of zero valent iron nanoparticles (NZVI) using three plant extracts and their efficient application for removal of Cr(VI) from aqueous solutions

In the present study, NZVI particles were synthesized from the plant extracts including Rosa damascene (RD), Thymus vulgaris (TV), and Urtica dioica (UD). The FTIR arspectshowed that polyphenols, proteins and organic acids which serve as reducing and stabilizing agents play a significant role in the synthesis of NPs and reduce the possibility of aggregation of NPs compared to chemical techniques of NPs synthesis. The amount and type of compounds in plant extracts affect the structure and also agglomeration of NPs after adsorption process. Based on the results, the highest removal efficiency occurred at pH 2. With increase in contact time and amount of dose, the percentage removal increases. Inversely, increase of initial concentration of Cr(VI) decreases the removal efficiency of the contaminant. These nanoparticles have a high adsorption capacity. Accordingly, by applying a dose of 0.2 g/l and contact time of 10 min, the three NPs yielded >90% removal efficiency. Also, for 1 min contact time, the percentage removal was 94.87%, 83.48% and 86.8% for RD-Fe, UD-Fe and TV-Fe, respectively. By an increase to 25 min, the removal percentage reached to 100% for TV-Fe and UD-Fe. Moreover, 30 min was required to remove Cr(VI) completely by RD-F.     

Preparation of mono-dispersed carbonaceous spheres via a hydrothermal process

Mono-dispersed carbonaceous spheres (CS) with a narrow size distribution were synthesized via hydrothermal treatment of glucose. The effects of hydrothermal temperature and time, glucose concentration and pH value of solution were investigated in detail. Structures and surface properties of as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Induced coupled plasma emission spectroscopy (ICP), thermogravimetric analysis/differential scanning calorimetry (TG/DSC), Nitrogen adsorption/desorption and Fourier transformed infrared spectroscopy (FTIR). The results showed that the production yield of CS increased from 2.1 to 32% with increasing the temperature from 160 to 180 °C, and the average size increased from 0.23 to 0.95 μm with extending the hydrothermal time from 8 to 16 h. pH value of the starting solution showed an evident effect on the morphology of CS via affecting the decomposition products of glucose. CS could be obtained when the pH value of starting solution was less than 12, but further increasing the pH value to 13–14 led to the formation of lumpy aggregations of carbon rather than spherical CS. The CS prepared under pH 6 and 9 showed good adsorption capacity for Methylene blue (MB), which was attributed to their relatively high specific surface area.     

(101)-oriented ZnO nanoparticles fabricated in Si (100) by Zn ion implantation and thermal oxidation

ZnO nanoparticles (NPs) embedded in Si (100) substrate have been created by Zn ion implantation and post thermal annealing in oxygen atmosphere. Several techniques have been employed to investigate the formation of Zn NPs and their thermal evolution at elevated temperatures. Grazing X-ray diffraction results clearly show that ZnO NPs are effectively formed after 600 °C annealing, and they show a (101) preferential orientation. Cross-sectional transmission electron microscopy observations confirm that ZnO NPs with a narrow size distribution of 2–7 nm are formed within the near-surface region of about 35 nm in thickness. Photoluminescence measurement displays a strong emission band centered at 387 nm in the sample annealed at 600 °C.