Solvothermal synthesis and analysis of Bi1−xSbx nanoparticles

Bismuth-antimony alloy nanoparticles have been synthesized by a facile solvothermal method using N,N-dimethylformamide and ethylene glycol as solvent/reducing agent; BiCl₃, SbCl₃ and Bi(NO₃)₃ as precursors; and citric acid as a surface modifier/stabilizing agent. The particle size and size distribution of Bi nanoparticles were analyzed as a function of the synthesis conditions: molar ratio of precursor to surfactant, precursor concentration and reducing agent. Synthesis of Sb and Bi_0.88Sb_0.12 under similar conditions was also investigated. The phase purity of nanoparticles was confirmed from X-ray diffraction and thermogravimetry and the nanoparticle morphology was investigated by transmission electron microscopy. A case study of Bi nanoparticles with detailed analysis of the particle morphology and size distribution of the nanoparticles is reported.     

Photochemical synthesis of Bi2Se3 nanosphere and nanorods

A photochemical reaction route was developed to synthesize bismuth selenide (Bi₂Se₃) nanoparticles and nanorods. In an aqueous solution, bismuth nitrate (Bi(NO₃)₃) reacted with sodium selenosufate in the presence of reducing agent and complexing agent, and the dispersed Bi₂Se₃ nanoparticles were obtained with the average size of 35 nm. The nanorods were prepared via an alumina template route in the same solution. We carried out experiments to study the formation mechanism in the morphology control of the products and found that series of factors played an effective role including the irradiation time, pH value, the reducing agents and the species of complexing agents. The products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM).     

Rapid biologically one-step synthesis of stable bioactive silver nanoparticles using Osage orange (Maclura pomifera) leaf extract and their antimicrobial activities

Synthesis of nanoparticles by using natural products as reducing and stabilizing agents have been widely used in various fields especially medicine, primarily because of its lower cost, simplicity, and less toxic byproducts. In the present work, silver nanoparticles (Ag NPs) were rapidly synthesized from silver nitrate in a green one-step synthesis by the aqueous extracts of Osage orange (Maclura pomifera) leaf as a reducing and stabilizing agent simultaneously. The effects of pH, extract quantity, and silver salt concentration were investigated to determine the optimum conditions of green synthesis of Ag NPs. The synthesized Ag NPs were characterized by different techniques including UV–Visible (UV–Vis) absorption spectroscopy, X-ray diffraction (XRD), Fourier transform Infrared (FT-IR) Spectroscopy, and Transmission Electron Microscopy (TEM). The Ag NPs showed surface plasmon resonance centered at 415?nm. The XRD pattern and TEM analysis revealed spherical, stable, and uniform Ag NPs with the average particle size of about 12?nm. The FT-IR spectroscopy showed that mainly hydroxyl functional groups, as both the reducing and stabilizing agent are responsible for silver nanoparticles synthesis. The antimicrobial activity of the synthesized Ag NPs showed a significant microbicidal effect on all clinical isolates especially, Gram-negative bacteria and fungi. These results suggest that such stable and uniform Ag NPs can be synthesized rapidly and simply for clinical as well as pharmaceutical applications.     

The use of de-aggregating agents in ZnSe mechanochemical synthesis

Conventional mechanochemical synthesis of zinc selenide, ZnSe nanoparticles was performed in a planetary ball mill by high-energy milling of zinc (Zn) and selenium (Se) powders with the de-aggregating agents ZnCl₂ and phthalic acid (aromatic dicarboxylic acid, C₈H₆O₄). Physical–chemical and optical properties of the prepared ZnSe nanoparticles were studied and compared. The mechanochemically synthesized products were characterized by X-ray diffraction analysis (XRD) that confirmed the presence of cubic-Stilleite and hexagonal ZnSe phases after 18, 25, 30, 40, 45 and 50 min of milling with various amounts of the added de-aggregating agents. Size of crystallites calculated from XRD patterns was from 20 to 31 nm for cubic ZnSe prepared with ZnCl₂. For ZnSe synthesized with phthalic acid the crystallite size ranged from 16 to 73 nm. Size, phase composition, morphology, and crystallinity of ZnSe nanoparticles were studied by transmission electron microscopy (TEM) and selected area electron diffraction (SAED). Photoluminescence spectra (PL) at room temperature have shown a broad red emission bands, and the presence of de-aggregating agent has altered the intensity of the PL signal as well.     

Microbial Synthesis of Multishaped Gold Nanostructures

The development of methodologies for the synthesis of nanoparticles of well‐defined size and shape is a challenging one and constitutes an important area of research in nanotechnology. This Full Paper describes the controlled synthesis of multishaped gold nanoparticles at room temperature utilizing a simple, green chemical method by the interaction of chloroauric acid (HAuCl₄ · 3H₂0) and cell‐free extract of the fungal strain Rhizopus oryzae. The cell‐free extract functions as a reducing, shape‐directing, as well as stabilizing, agent. Different shapes of gold nanocrystals, for example, triangular, hexagonal, pentagonal, spherical, spheroidal, urchinlike, two‐dimensional nanowires, and nanorods, are generated by manipulating key growth parameters, such as gold ion concentration, solution pH, and reaction time. The synthesized nanostructures are characterized by UV/Vis and Fourier‐transform infrared spectroscopy, transmission electron microscopy, and energy dispersive X‐ray analysis studies. Electron diffraction patterns reveal the crystalline nature of the nanoparticles and a probable mechanism is proposed for the formation of the different structural entities.     

Preparation and characterization of Cu(In,Ga)Se2 films from nanosized alloy precursors

CuInSe₂ films were successfully prepared from the nanoparticles that were synthesized via the chemical reduction reaction. In the chemical reduction process using ethylene glycol as the solvent and NaBH₄ as a reducing agent, CuIn and Cu₂In phases were detected. Upon increasing the molar ratio of the reducing agent to the metal ions, Cu₁₁In₉ and In were formed and coexisted with Cu–In alloys. The obtained nanoparticles were utilized in pastes for coating Cu(In,Ga)Se₂ films. The XRD results and Raman spectra elucidated the formation mechanism. During the selenization process, InSe and Cu_2?xSe were produced and then reacted with each other to yield CuInSe₂. Cu(In,Ga)Se₂ was also prepared using the nanoparticles via the reduction reaction. In the route developed herein not only was the temperature of the synthesis of the chalcopyrite compounds reduced to 450 °C, but also the phases of the powders that were used in the synthesis of Cu(In,Ga)Se₂ films were controlled.     

Facile and green synthesis of cobalt oxide nanoparticles using ethanolic extract of Trigonella foenumgraceum (Fenugreek) leaves

Cobalt oxide nanoparticles (Co₃O₄ NPs) were successfully synthesized using ethanolic extract of Trigonella foenumgraceum L. (fenugreek) leaves as a green, potentially low cost, and easily biosynthesized method. The organic bioactive compounds present in fenugreek leaves extract acted as both reducing agents and stabilizing agents for synthesizing metal NPs from cobalt chloride hexahydrate as a precursor. As evidence from UV/Visible spectroscopy, energy dispersive spectroscopy (EDS), and X-ray diffraction analysis (XRD) studies, high alkaline pH was found favorable for the preparation of pure and crystallized single-phase Co₃O₄ NPs. The interaction of biomolecules from fenugreek leaves extract with Co₃O₄ NPs was defined by Fourier transform infrared spectroscopy (FTIR) analysis and X-ray photoelectron spectroscopy (XPS). The hydrodynamic size and surface charge of the biosynthesized NPs were measured using light-scattering (DLS) and zeta potential analyses; revealed the formation of negative charged Co₃O₄ NPs with uniform hydrodynamic size distribution. According to transmission electron microscopy (TEM) analysis, quasi-spherical Co₃O₄ NPs were synthesized with an average size of 13.2 nm under the modified condition of pH 12 and reaction time of 2 h through inexpensive, environmental friendly benign synthesis process without the use of any additional toxic chemical.     

One step synthesis of silica-coated nanoparticles at room temperature and their luminescence properties

A novel one-step preparation method for core-shell CdS/SiO₂ nanoparticles was proposed using 3-mercaptopropyl-trimethoxysilane (MPS) as stabilizing agent in MeOH, in which CdCl₂·2.5H₂O and Na₂S·9H₂O were used as the source of Cd and S, respectively. And the photostability of the nanoparticles was further investigated. The morphology and structure of products was characterized by scanning probe microscope and FT-IR spectra, respectively. Furthermore, the influences of Zn and Cu doped in the products, individually, on the fluorescence property were discussed. The results showed that the products were ball-shaped and silica-coated with a uniform size, the spectra of Zn-doped was blue shifted, however, the spectra of Cu-doped was red shifted, the core-shell CdS/SiO₂ nanoparticles was more steady compared with thioglycolic acid-capped CdS nanoparticles.     

Synthesis of Starch-Stabilized Silver Nanoparticles and Their Antimicrobial Activity

In this study, silver nanoparticles were prepared using silver nitrate as the metal precursor, starch as protecting agent, and sodium borohydride (NaBH₄) as a reducing agent by the chemical reduction method. The formation of the silver nanoparticles was monitored using ultraviolet-visible absorption spectroscopy, cyclic voltammetry, and particle size analyzer and characterized by transmission electron microscopy (TEM) and x-ray diffraction (XRD). Synthesis of nanoparticles were carried out by varying different parameters, such as reaction temperature, concentration of reducing agent, concentration of silver ion in feed solution, type and concentration of the stabilizing agent, and stirrer speed expressed in terms of particle size and size distribution. Dispersion destabilization of colloidal nanoparticles was detected by Turbiscan. It was observed that size of the starch stabilized silver nanoparticles were lower than 10 nm. The microbial activity of synthesized silver nanoparticles was examined by modified Kirby-Bauer disk diffusion method. Silver nanoparticles were tested for their antibacterial activity against Gram negative bacteria such as Escherichia coli, Pseudomonas aeruginosa, and Gram positive bacteria such as Staphylococcus aureus and Staphylococcus epidermidis. High bacterial activity was observed at very low concentrations of silver (below 1.39 μg/ml). The antifungal activity of silver nanoparticles has been assayed against Candida albicans.     

Facile synthesis and characterization of CdTiO<Subscript>3</Subscript> nanoparticles by Pechini sol–gel method

In this work, CdTiO₃ nanoparticles were synthesized through reaction between Cd(CH₃COO)₂.2H₂O, Ti(OC₄H₉)₄, trimesic acid as a new chelating agent and ethanol as solvent by Pechini sol–gel method. X-ray diffraction (XRD) patterns showed that CdTiO₃ nanostructures have rhombohedral structure with diameter of about 35.61 nm. The structure, morphology and size of CdTiO₃ nanoparticles were characterized by FT-IR, XRD, SEM and EDAX. The optical properties of the products were studied by DRS. Based on the results of experiments, it was found that temperature and time of calcination, pH and the solvent of reaction are important parameters for formation of CdTiO₃ nanoparticles. Utilizing trimesic acid (benzene-1,3,5-tricarboxylic acid) as a new chelating agent for preparation of CdTiO₃ nanostructures was initiative of this work.     

Synthesis and Characterization of Fe-Doped CdSe Nanoparticles as Dilute Magnetic Semiconductor

Cd_1?x Fe _x Se (0??x??0.1) nanoparticles were synthesized by hydrothermal method. The solubility limit of Fe in CdSe nanoparticles was found to be less than 6?% as obtained from X-ray diffraction (XRD) study. With the increase in doping concentration at and above it, secondary phase of FeSe₂ starts appearing. The presence of Cd, Se, and Fe has been confirmed by energy dispersive X-ray spectroscopy (EDS). The increase in band gap value has been confirmed by UV-visible spectra and the variation in emission intensity of photoluminescence (PL) measurements further indicates the incorporation of Fe in CdSe nanoparticles. Transmission electron microscopy (TEM) reveals the spherical nature of synthesized nanoparticles, and the particle size decreases with increasing Fe doping concentration. Fourier transform Infrared spectra (FTIR) confirm the capping of sodium dodecyl sulfate (SDS) surfactant on pure and Fe-doped CdSe nanoparticles. The synthesized nanoparticles show room-temperature ferromagnetic behavior, and the saturation magnetization value was found to increase with Fe doping concentration.     

One-pot synthesis of CuFeSe2 cuboid nanoparticles

Ternary semiconducting CuFeSe₂ nanocrystals of a particular shape and size were successfully synthesized using a cost-effective and simple one-pot chemical route. X-ray powder diffraction and field emission scanning electron microscopy results indicated that the as-synthesized CuFeSe₂ comprised cuboid nanoparticles with dimensions of 50–150 nm as well as a tetragonal phase. Elemental analysis yielded an atomic ratio of Cu:Fe:Se of 1:1.06:2.17. The synthesis temperature and the solvent octadecylamine were significant in determining the structural phases and morphologies of the final products. The optimal condition for synthesizing the tetragonal CuFeSe₂ phase with cuboid nanoparticles was a reaction temperature of 200 °C for 1 h in octadecylamine solvent. A possible mechanism of the formation of ternary CuFeSe₂ nanoparticles with controllable shapes is discussed.     

Synthesis of stable dispersion of copper nanoparticles in a water-in-supercritical carbon dioxide using polydimethylsiloxane as the stabiliser

This study reportes the synthesis of stable dispersion copper nanoparticles by chemical reduction of copper chloride (CuCl₂) in a water-in-supercritical carbon dioxide medium using sodium borohydrate (NaBH₄) as a reducing agent, polydimethylsiloxane as the stabiliser and sodium bis(2-ethylhexyl)sulphosuccinate (AOT) as co-surfactant at temperature 40°C and pressure in the range 2000–2400?psi. UV–visible spectroscopy exhibits a typical emission peak at 560–590?nm for Cu nanoparticles. By changing the reaction pressure and the stabiliser concentration, the size and the shape of the copper nanoparticles could be easily controlled. The X-ray diffraction pattern reveals that the Cu nanoparticles are formed in the range 4–8?nm, which is consistent with the transmission electron microscopy images.     

Facile fabrication of ultrasmall and uniform copper nanoparticles

Ultrasmall and uniform copper nanoparticles were synthesized through a trace-level ethylenediaminetetraacetic acid (EDTA)-assisted wet chemical route in which Cu(OH)₂ colloid, KBH₄ and polyvinyl pyrrolidone (PVP) were used as the Cu source, the reducing agent, and the protective agents, respectively. The copper nanoparticles exhibit a spherical morphology with a narrow size distribution, a uniform shape, and the average diameter of ca. 4 nm. The presence of trace EDTA is indispensable for the preparation of ultrasmall and uniform copper nanoparticles. EDTA concentration directly influences the copper nanoparticle size and uniformity. As EDTA concentration decreases, the size of the copper nanoparticles decreases, whereas the uniformity increases. The possible formation mechanism of ultrasmall and uniform copper nanoparticles was determined according to experimental results.     

Studies of the factors effecting the preparation of heterogeneous platinum-based catalyst on silica supports

Pt nanoparticles with an average size of ∼3 nm were successfully immobilized on the surface of SiO₂ functionalized with -NH₂ and -SH groups through chemical reduction process using polyvinylpyrrolidone as a stabilizer and different reducing agents. The effects of molecular weight of polyvinylpyrrolidone, molar ratio of reducing agent to Pt salt, type of reducing agent on the size and degree of agglomeration of Pt nanoparticles on the SiO₂ surface were investigated. The X-ray diffraction and transmission electron micrograph analyses were performed to identify the product phase, size and morphology of immobilized Pt onto SiO₂. UV-vis analysis was also conducted to identify the degree of reduction of Pt ions. The Pt-SiO₂ nanocomposite prepared from both NH₂- and SH-functionalized SiO₂ exhibited similar behavior. The number of immobilized Pt nanoparticles and their average size was increased with polyvinylpyrrolidone concentration while the number of immobilized Pt was decreased with its molecular weight.     

Synthesis of Se nanoparticles by using TSA ion and its photocatalytic application for decolorization of cango red under UV irradiation

In this study, we describe a size-controlled synthesis of selenium nanoparticles based on the reduction of selenious acid (H₂SeO₃) by UV-irradiated tungstosilicate acid (H₄SiW₁₂O₄₀, TSA) solution which serves both as reducing reagent and stabilizer. The nanoparticles are characterized by ultraviolet-visible spectroscopy (UV-vis), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction analysis (XRD), X-ray photoelectron spectroscopy (XPS), the Raman spectra, transmission electron microscopy (TEM) and Zetasizer, respectively. The characteristic catalytic behavior of the Se nanoparticles is established by studying the decolorization of cango red in the presence of UV light. It is obvious that selenium catalyzes the reaction efficiently. The results show that the rate of dye decolorization varies linearly with the nanoparticle concentration and the rate of dye decolorization decreases with the size of the Se nanoparticles increasing.     

室温条件下纳米银的温和制备和形貌调控

目的 探究室温条件下不同还原剂以及其他实验助剂在化学还原纳米银过程中对其颗粒粒径、尺寸分布和形貌的影响。方法 以抗坏血酸为还原剂,聚乙烯吡咯烷酮（PVP）为分散剂,柠檬酸钠为保护剂和第2还原剂,选择葡萄糖和硼氢化钠作对照,在室温下通过化学还原的方法来制备纳米银颗粒。通过马尔文激光粒度仪、紫外–可见光谱（UV–vis）、透射电镜（TEM）等对所制备纳米银进行表征。结果 采用抗坏血酸作为还原剂时,通过调控抗坏血酸体积（0.2 mL）,固定柠檬酸钠和PVP体积分别为0.5、0.6 mL,制备出粒径较小（平均粒径为56 nm）且尺寸分布较均一的球形纳米银;采用葡萄糖和硼氢化钠作还原剂时纳米银颗粒尺寸过大（平均粒径分别为216nm和189nm）。结论 采用抗坏血酸作为还原剂,调控柠檬酸钠、PVP等实验参数在最佳范围,更容易制备出球形度好、粒径小的均匀纳米银溶液。     

Novel synthesis of nanocrystalline CeO2 by mechanochemical and water-in-oil microemulsion methods

Nanocrystalline cerium dioxide (CeO₂) had been synthesized by two different methods which were mechanochemical and water-in-oil microemulsion. Effects of synthesis conditions on properties of nanocrystalline cerium dioxide were investigated. X-ray diffraction (XRD) was used to characterize the phase and crystallite size of synthesized cerium dioxide nanoparticles. XRD results showed that face centered cubic CeO₂ nanoparticles with crystallite size in nanometer scale were formed. The crystallinity increased with increasing annealing temperature. The average specific surface area of the particles was probed using gas adsorption-desorption measurements. The average particles size was calculated from the specific surface area and was determined to be 5.2 nm for microemulsion samples and 6.9 nm for mechanochemical samples. These results showed that properties of synthesized cerium dioxide could be tailored by adjusting the synthesis conditions.     

Synthesis of TbMnO3 nanoparticles via a polyacrylamide gel route

We report here the synthesis of TbMnO₃ nanoparticles via an acrylamide gel route. XRD, TG analysis, DSC analysis, and FTIR spectroscopy are combinatively used to investigate the thermal decomposition process of precursor xerogels and the formation of TbMnO₃ phase. It is demonstrated that high-phase-purity TbMnO₃ nanoparticles can be prepared by using different chelating agents at a sintering temperature of 800 °C. SEM observation and XRD analysis reveal that the particle size and morphology of the products have a dependence on the chelating agent. The particles prepared using citric acid as the chelating agent appear to be regularly spherical in shape and highly uniform in size with a diameter of ～67 nm, while the sample prepared by using the chelating agent EDTA mainly consists of sphere-, ellipsoid-, and rod-like particles and exhibits a relatively broad particle size distribution with an average particle size centered around 115 nm. The use of a combination of citric acid and EDTA generally results in sphere- and ellipsoid-like particles with an average particle size between those of the samples prepared separately by using the two chelating agents.     

Biosynthesised AgCl NPs using Bacillus sp. 1/11 and evaluation of their cytotoxic activity and antibacterial and antibiofilm effects on multi‐drug resistant bacteria

Silver nanoparticles (AgNPs) have attracted the attention of researchers due to their properties. Biological synthesis of AgNPs is eco‐friendly and cost‐effective preferred to physical and chemical methods, which utilize environmentally harmful agents and large amounts of energy. Microorganisms have been explored as potential biofactories to synthesize AgNPs. Bacterial NP synthesis is affected by Ag salt concentration, pH, temperature and bacterial species. In this study, Bacillus spp., isolated from soil, were screened for AgNP synthesis at pH 12 with 5 mM Ag nitrate (AgNO₃) final concentration at room temperature. The isolate with fastest color change and the best ultraviolet‐visible spectrum in width and height were chosen as premier one. AgNO₃ and citrate salts were compared in terms of their influence on NP synthesis. Spherical Ag chloride (AgCl) NPs with a size range of 35–40 nm were synthesized in 1.5 mM Ag citrate solution. Fourier transform infrared analysis demonstrated that protein and carbohydrates were capping agents for NPs. In this study, antimicrobial and antitumor properties of the AgNP were investigated. The resulting AgCl NPs had bacteriostatic activity against four standard spp. And multi‐drug resistant strain of Pseudomonas aeruginosa. These NPs are also cytotoxic to cancer cell lines MCF‐7, U87MG and T293.Inspec keywords: silver compounds, nanoparticles, nanomedicine, nanofabrication, particle size, biomedical materials, microorganisms, ultraviolet spectra, visible spectra, Fourier transform infrared spectra, proteins, macromolecules, antibacterial activity, tumours, cancer, cellular biophysics, toxicologyOther keywords: citrate salts, spherical Ag chloride, particle size, Ag citrate solution, Fourier transform infrared analysis, protein, carbohydrates, capping agents, antitumour properties, bacteriostatic activity, Pseudomonas aeruginosa, multidrug resistant strain, cancer cell lines MCF‐7,U87MG, size 35 nm to 40 nm, temperature 293 K to 298 K, AgCl, ultraviolet‐visible spectrum, colour change, room temperature, Ag nitrate final concentration, soil, bacterial species, temperature effect, pH, Ag salt concentration, biofactories, microorganisms, environmentally harmful agents, chemical methods, physical methods, antibacterial properties, electrical properties, mechanical properties, silver nanoparticles, multidrug resistant bacteria, antibiofilm effects, antibacterial effects, cytotoxic activity, Bacillus sp. 1/11, biosynthesised AgCl NPs