Size-controlled synthesis of alumina nanoparticles from aluminum alkoxides

Aluminum oxide nanoparticles were prepared by the hydrolysis of aluminum oxide alkoxides followed by calcinations, in the presence of surface stabilizing agents, such as Na(AOT) molecules. The size of alumina precursors (bohemite) was 20-30 nm, yielding aluminum oxide particles with an average size of 80 nm after calcinations at 1200 °C. The shape of the α-alumina nanoparticles was mainly spherical and the high temperature inhibited the formation of the hexagonal crystals. The introduction of Na(AOT) during the appropriate processing step, had the effect of controlling the size of the particles, the degree of aggregation and the particles shapes.     

Synthesis of size tuneable cadmium sulphide nanoparticles from a single source precursor using ammonia as the solvent

Size tuneable cadmium sulphide nanoparticles of a few nanometres in size were prepared by thermolysis of a single source precursor of cadmium xanthates with variable carbon chain length (Cd(ROCS₂)₂, where R denotes -C₂H₅, -C₄H₉, -C₈H₁₇ and -C₁₂H₂₅, respectively) in an ammonia solution. The particle size, morphology and crystallinity of these nanoparticles were characterized using X-ray powder diffractometry, transmission electron microscopy, and nitrogen adsorption/desorption techniques. The results show that hexagonal CdS nanoparticles can be produced by thermolysis of cadmium alkyl xanthate in an ammonia solution at a temperature as low as 100 °C. The size of CdS particles (between 5.60 nm and 3.71 nm) decreases with increasing length of carbon chain in the precursor, as further confirmed by UV-visible and fluorescence spectrophotometric measurements. The size tuning mechanism of CdS from cadmium alkyl xanthate is also discussed.     

IF-WS2 nanoparticles size design and synthesis via chemical reduction

An innovative synthesis of inorganic fullerene-like disulfide tungsten (IF-WS₂) nanoparticles was developed using a chemical reduction reaction in a horizontal quartz reactor. In this process, first tungsten trisulfide (WS₃) was formed via a chemical reaction of tetra thiotungstate ammonium ((NH₄)₂WS₄), polyethylene glycol (PEG), and hydrochloric acid (HCl) at ambient temperature and pressure. Subsequently, WS₃ was reacted with hydrogen (H₂) at high temperature (1173-1373 K) in a quartz tube. The produced WS₂ nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), and transmission electron microscopy (TEM). The characterization results indicated that the high-purity (100%) IF-WS₂ nanoparticles were produced. Moreover, addition of surfactant (PEG) and higher operating temperature (1173-1373 K) decreased the particles agglomeration, and consequently led to the reduction of average diameter of WS₂ particles in the range of 50-78 nm. The developed method is simple, environmentally compatible, and cost-effective in contrast to the conventional techniques.     

Preparation and characterization of nanocrystallite size cuprous oxide

Uniform spheres of nanocrystallite size cuprous oxide particles have been prepared by a simple polyol process using cupric nitrate as a precursor in ethylene glycol. As synthesized compound was dried at 333 K in a vacuum oven and characterized by XRD, FT-IR and SEM techniques. The crystallite size of the cuprous oxide calculated from Scherer's formula was found to be ∼11 nm.     

CeF3 nanoparticles: synthesis and characterization

CeF₃ nanoparticles 5-10 nm in size were prepared using the polyol method. CeCl₃ and HF were heated up in ethylene glycol. At a temperature of 180 °C crystalline CeF₃ nanoparticles were formed. The material was washed with ethanol, centrifugated and dried. The particles were characterized by EDX, XRD and TEM.     

A simple route to large-scale production of tungsten trioxide nanoparticles

Tungsten trioxide particles in high yield were prepared via a simple solid evaporation route with ammonium paratungstate hydrate as precursor and Ar gas as carrier gas. Detailed characterization by scanning electron microscopy has shown that increasing carrier gas flow rate promotes morphological evolution from large and irregular semi-spherical particles to non-agglomerated quasi-spherical particles, and finally to single-crystalline nanoparticles with an average diameter of 60 nm. The adsorption activity of the tungsten trioxide particles is size-dependent and increased with decreasing particle size. The present method could readily produce large-scale tungsten trioxide nanoparticles with ideal adsorption performance, and can be utilized to fabrication of various semiconductor oxides with advanced properties.     

Dendrigraft polymer-based synthesis of silver nanoparticles showing bright blue fluorescence

A novel method is reported here for the synthesis of optically clear and stable colloidal solutions of silver nanoparticles. According to size they show different colours depending upon their plasmonic absorption frequencies. The materials have been synthesized at room temperature by chemical reduction of silver ions (silver nitrate) coordinated with dendrigraft polymer, polyethyleneimine (PEI) using formaldehyde in aqueous medium. UV-vis absorption and transmission electron microscopy (TEM) studies show single-band absorption with peak maximum at 354 nm for ∼3 nm sized particles, whereas a side band at ∼400 nm was observed when the particle size increased to ∼20 nm. Highly narrow particle size distribution was observed in case of samples having ∼3 nm size silver particles and also the process of reduction could be completed within minutes. More interestingly, the 3-nm sized particles showed strong blue (474 nm) fluorescence under UV excitation. Thin films of all synthesized samples were prepared on silica substrate by fine spray coating technique.     

Synthesis and anti-bacterial activity of Cu, Ag and Cu-Ag alloy nanoparticles: A green approach

Metallic and bimetallic nanoparticles of copper and silver in various proportions were prepared by microwave assisted chemical reduction in aqueous medium using the biopolymer, starch as a stabilizing agent. Ascorbic acid was used as the reducing agent. The silver and copper nanoparticles exhibited surface plasmon absorption resonance maxima (SPR) at 416 and 584 nm, respectively; while SPR for the Cu-Ag alloys appeared in between depending on the alloy composition. The SPR maxima for bimetallic nanoparticles changes linearly with increasing copper content in the alloy. Transmission electron micrograph (TEM) showed monodispersed particles in the range of 20 ± 5 nm size. Both silver and copper nanoparticles exhibited emission band at 485 and 645 nm, respectively. The starch-stabilized nanoparticles exhibited interesting antibacterial activity with both gram positive and gram negative bacteria at micromolar concentrations.     

Green synthesis of zinc oxide nanoparticles by aloe barbadensis miller leaf extract: Structure and optical properties

Biological methods for nanoparticle synthesis using microorganisms, enzymes, and plants or plant extracts have been suggested as possible ecofriendly alternatives to chemical and physical methods. In this paper, we report on the synthesis of nanostructured zinc oxide particles by both chemical and biological method. Highly stable and spherical zinc oxide nanoparticles are produced by using zinc nitrate and Aloe vera leaf extract. Greater than 95% conversion to nanoparticles has been achieved with aloe leaf broth concentration greater than 25%. Structural, morphological and optical properties of the synthesized nanoparticles have been characterized by using UV-Vis spectrophotometer, FTIR, Photoluminescence, SEM, TEM and XRD analysis. SEM and TEM analysis shows that the zinc oxide nanoparticles prepared were poly dispersed and the average size ranged from 25 to 40 nm. The particles obtained have been found to be predominantly spherical and the particle size could be controlled by varying the concentrations of leaf broth solution.     

Nano-sized manganese oxide particles prepared by low-pressure spray pyrolysis using FEAG process

Nano-sized manganese oxide particles were prepared by low-pressure spray pyrolysis using the new type of liquid aerosol generator called as FEAG process. The particles prepared from polymeric precursors spray solution with organic additives had large size, hollow and fractured morphologies due to the gas evolution from the decomposition of the organic additives. The precursor particles with micron size, hollow and thin wall structures turned to nano-sized manganese oxide particles after post-treatment at temperatures of 700 and 800 °C. The optimum concentrations of citric acid (CA) and ethylene glycol (EG) to prepare the nano-sized manganese oxide particles by spray pyrolysis using the FEAG process were 0.3 M each. The manganese oxide particles prepared from the polymeric precursors spray solutions with high concentrations of CA and EG had spherical shape and porous morphologies.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.     

Vapor-phase synthesis of a solid precursor for α-alumina through a catalytic decomposition of aluminum triisopropoxide

A new solid precursor, hydrous aluminum oxide, for α-alumina nanoparticles was prepared by thermal decomposition of aluminum triisopropoxide (ATI) vapor in a 500 mL batch reactor at 170-250 °C with HCl as catalyst. The conversion of ATI increased with increasing temperature and catalyst content; it was nearly complete at 250 °C with the catalyst at 10 mol% of the ATI. The obtained precursor particles were amorphous, spherical and loosely agglomerated. The primary particle size is in the range 50-150 nm. The ignition loss of the precursor was 24%, considerably lower than 35% of Al(OH)₃, the popular precursor for alumina particles. Upon calcination of the precursor at 1200 °C in the air with a heating rate of 10 °C/min and a holding time of 2 h, the phase was completely transformed into α. The spherical particles composing the precursor turned worm-like by the calcination probably due to sintering between neighboring particles. The surface area equivalent diameter of the resulting α-alumina was 75 nm.     

Hydroxy propyl cellulose capped silver nanoparticles produced by simple dialysis process

Silver (Ag) nanoparticles (∼6 nm) were synthesized using a novel dialysis process. Silver nitrate was used as a starting precursor, ethylene glycol as solvent and hydroxy propyl cellulose (HPC) introduced as a capping agent. Different batches of reaction mixtures were prepared with different concentrations of silver nitrate (AgNO₃). After the reduction and aging, these solutions were subjected to ultra-violet visible spectroscopy (UVS). Optimized solution, containing 250 mg AgNO₃ revealed strong plasmon resonance peak at ∼410 nm in the spectrum indicating good colloidal state of Ag nanoparticles in the diluted solution. The optimized solution was subjected to dialysis process to remove any unreacted solvent. UVS of the optimized solution after dialysis showed the plasmon resonance peak shifting to ∼440 nm indicating the reduction of Ag ions into zero-valent Ag. This solution was dried at 80 °C and the resultant HPC capped Ag (HPC/Ag) nanoparticles were studied using transmission electron microscopy (TEM) for their particle size and morphology. The particle size distribution (PSD) analysis of these nanoparticles showed skewed distribution plot with particle size ranging from 3 to 18 nm. The nanoparticles were characterized for phase composition using X-ray diffractrometry (XRD) and Fourier transform infrared spectroscopy (FT-IR).     

Spontaneous formation of silver nanoparticles on polymeric supports

Silver nanoparticles with a size range of 2-4 nm were prepared on polyethylene glycol-coupled 2-chlorotrityl resins without using any reducing agents. In contrast to the polyol process, silver nanoparticles were simply reduced in the tetrahydrofuran/chloroform system on the resin without using any alcohols, and the resulting silver nanoparticles exhibited a uniform size distribution. The polyethylene glycol spacer on the resin played an important role in obtaining silver nanoparticles, probably acting as a polydentate-chelating agent for the silver ions.     

Biological synthesis of very small silver nanoparticles by culture supernatant of Klebsiella pneumonia: The effects of visible-light irradiation and the liquid mixing process

This study has investigated different visible-light irradiation's effect on the formation of silver nanoparticles from silver nitrate using the culture supernatant of Klebsiella pneumonia. Our study shows that visible-light emission can significantly prompt the synthesis of silver nanoparticles. Also, the study experimentally investigated the liquid mixing process effect on silver nanoparticle synthesis by visible-light irradiation. This study successfully synthesized uniformly dispersed silver nanoparticles with a uniform size and shape in the range of 1-6 nm with an average size of 3 nm. Furthermore, the study investigated the mechanism of the reduction of silver ions by culture supernatant of K. pneumonia, and used X-ray diffraction to characterize silver chloride as an intermediate compound. Silver chloride was prepared synthetically and used as a substrate for the synthesis of silver nanoparticles by culture supernatant of K. pneumonia. The silver nanoparticles have been prepared from silver chloride during this investigation for the first time.     

Preparation and characterization of zinc sulfide nanoparticles under high-gravity environment

Nanosized ZnS particles were prepared under high-gravity environment generated by the rotating packed bed reactor (RPBR) using zinc nitrate solution and hydrogen sulfide gas as raw materials. The effects of experimental conditions such as reactant concentration, reaction temperature, rotating speed of the RPBR and aging time, on the preparation of nanosized ZnS particles were investigated. A set of suitable operating parameters (the aging time of 48 h, concentration of zinc nitrate of 0.1 mol/l, reaction temperature of 45 °C and rotating speed of the RPBR of 1500-1800 rotation/min) for the preparation of nanosized ZnS were recommended. Under these optimum conditions, well-dispersed ZnS nanoparticles was obtained. The crystal structure, optical properties, size and morphology of the product were also characterized by XRD, UV-Vis spectrophotometer, and TEM, respectively. Results indicate that the prepared ZnS has a good absorption for light in the wavelength range of 200-330 nm. XRD analysis also shows the prepared ZnS is in a sphalerite crystal phase. The process has great potential of commercialization.     

Preparation and electrocatalytic activity of tungsten carbide and titania nanocomposite

Tungsten carbide and titania nanocomposite was prepared by combining a reduced-carbonized approach with a mechanochemical approach. The samples were characterized by X-ray diffraction, transmission electron microscope under scanning mode and X-ray energy dispersion spectrum. The results show that the crystal phases of the samples are composed of anatase, rutile, nonstoichiometry titanium oxide, monotungsten carbide, bitungsten carbide and nonstoichiometry tungsten carbide, and they can be controlled by adjusting the parameters of the reduced-carbonized approach; tungsten carbide particles decorate on the surface of titania support, the diameter of tungsten carbide particle is smaller than 20 nm and that of titania is around 100 nm; the chemical components of the samples are Ti, O, W and C. The electrocatalytic activity of the samples was measured by a cyclic voltammetry with three electrodes. The results indicate that the electrocatalytic activities of the samples are related to their crystal phases and the property of electrolyte in aqueous solution. A synergistic effect between titania and tungsten carbide is reported for the first time.     

Synthesis of nanometal oxides and nanometals using hot-wire and thermal CVD

We report the synthesis of nano-oxides of molybdenum, tungsten, and zinc. Molybdenum oxide (MoO₃) and tungsten oxide (WO_x) were produced by hot-wire CVD with molybdenum and tungsten filaments, respectively while zinc oxide (ZnO) was produced by thermal CVD. When high purity molybdenum wire was oxidized at ambient system atmosphere, nanorods and nanostraws of MoO₃ with length ranging from ∼ 20-80 nm and diameters ranging from ∼ 5-15 nm were produced. Also, the oxidation of the tungsten filament led to the deposition of tungsten oxide nanorods (10-25 nm diameter and 75-90 nm long) and nanospheres with diameters of ∼ 60 nm. Each oxide was reduced to its metallic form by annealing in a hydrogen environment to produce metallic nanoparticles. Nanorods and nanoribbons of ZnO with diameters ranging from 20-65 nm and lengths up to 2 μm were also produced.     

Preparation of nanosized titania by hydrolysis of alkoxide titanium in micelles

Nanosized titania particles, with typical particle sizes in the range of 30-50 nm have been synthesized using a microemulsion-mediated process. In this process, the aqueous cores of microemulsions have been used as constrained microreactors for the precipitation of titania precursor. The microemulsion was provided by a functionalized surfactant derived from the commercially available mixtures of sorbitol monooleate and polysorbate 80 (abbreviated as Span-Tween 80). The hydroxide particles, produced by the hydrolysis of the titanium tetraisopropoxide in the water droplets containing surfactant, were separated, dried, and calcined to form nanoparticles of TiO₂. The dependence of the size of the precipitated TiO₂ particles on various structure parameters of the microemulsion was studied in detail.     

Preparation and characterization of nanobiocomposites containing iron nanoparticles prepared from blood and coated with chitosan and gelatin

In this study, we report the preparation of magnetic iron nanoparticles (INPs) from goat blood using incineration method. FT-IR and XRD studies have confirmed that the prepared nanoparticles were INPs. These INPs were coated with a mixture of chitosan and gelatin to prepare INP-CG nanobiocomposite and the TEM picture of these composite particles has shown an average particle size of 80-300 nm. MRI scan exhibited magnetic property and VSM studies revealed a magnetic saturation of 18.97 emu/g. This may be used as a MRI contrast agent to enhance cellular imaging and as magnetic nanocarrier for targeted delivery of drugs in the diagnosis and treatment of cancer.