Synthesis, characterization, and optical properties of AuSe nanoalloys

A solution phase approach to synthesize a new metal-semiconductor nanocomposite, AuSe nanoalloy has been reported. The synthesis has been achieved through UV-photoactivation of preformed Au and Se nanoparticles in micelle. Non-ionic surfactant Triton X-100 was exploited as a micellar medium for effective fusion of gold and selenium particles under UV. Both physical and chemical studies have been performed to characterize the composition and morphology of the particles. UV-visible, TEM, SEM, XPS and AFM analyses were done for characterization purpose. The optical properties of nanocomposites have been substantiated through their interaction with a fluorescent probe, eosin in aqueous solution. The spectroscopic investigation of dye-metal-semiconductor assembly has been examined critically. It has been found that the dye experiences J and H types of aggregation on the surfaces of gold and selenium nanoparticles respectively. Again, the composition dependent change of the emission profile of the probe on different nanocomposite surfaces has been rationalized in accordance with the molecular dimerization of the dye.     

Synthesis of Yb nanoparticles by laser ablation of ytterbium target in sodium bis(2-ethylhexyl)sulfosuccinate reverse micellar solution

Surfactant-coated ytterbium nanoparticles were produced by Nd:YAG laser ablation of a Yb bulk target immersed in sodium bis(2-ethylhexyl)sulfosuccinate (AOT)/n-heptane micellar solution. In our experimental conditions, as highlighted by IR spectroscopy, AOT molecules are not decomposed by the intense laser pulses but play a pivotal role in the stabilisation of Yb nanoparticles. The formation of Yb nanoparticles in the liquid phase was monitored by UV-Vis spectroscopy whereas the Yb/AOT composites obtained by evaporation of the organic solvent were characterised by XPS and TEM. Data analysis consistently shows the presence of surfactant-coated, nearly spherical and non-interacting Yb nanoparticles of mean diameter of 3 nm.Moreover, the presence of bigger polycrystalline nanoparticles (about 30%) in coexistence with smaller mono crystalline ones indicates that, after the rapid formation of the pristine Yb nanoparticles from plume condensation, two processes effectively compete for their size distribution: nanoparticle agglomeration and surfactant adsorption.     

超声诱导CTAB/SDS溶液中纳米Pd粒子的形貌控制及对甲醛的电催化氧化

在十六烷基三甲基溴化铵(CTAB)-十二烷基硫酸钠(SDS)混合乙醇水溶液中,超声辐射PdCl2,合成了纳米Pd粒子,用XRD、TEM、选区电子衍射(SAED)、HRTEM和低温氮吸附-脱附等技术进行了表征,考察了CTAB/SDS组成对纳米粒子形貌的影响,纳米Pd粒子修饰玻碳电极对甲醛的电催化活性也通过循环伏安法进行了研究。结果表明:通过改变CTAB/SDS组成可以调控纳米Pd粒子的粒径和形貌;当CTAB与SDS物质的量之比为1∶1、超声反应60min时,得到呈多边形的纳米Pd粒子,粒径范围在10～20nm之间,比未添加表面活性剂样品的比表面积增大了14m2.g-1,对甲醛有较高的电催化活性。     

Aerosol phase generation of In-Se nanoparticles

Results on the generation and heat treatment of In-Se nanoparticles, made by heterogeneous condensation of selenium on indium nanoparticles synthesised via the evaporation/condensation route are reported. In-situ aerosol measurements are complemented with ex-situ analysis, to provide structural, morphological, and compositional information on the In-Se nanoparticles. Our results indicate that prior to heat treatment In-Se nanoparticles have a shape in the aerosol phase, similar to an asymmetric dumbbell. The bigger particle of the dumbbell structure is made up of amorphous Se, while the overall composition of the polycrystalline smaller particle is around InSe. The smaller particle has an intrinsic structure, and consists of different InSe-compounds, with a decreasing In content towards the shell. The shape of the In-Se nanoparticles is different in the aerosol phase and on the surface of the samples. The observed variety of particle sizes and shapes on the sample surface is shown to be partly due to the agglomeration of the aerosol phase binaries (i.e., dumbbells) via coalescence on the surface of the sample and wetting of the sample surface by the Se nanoparticles. These processes make the bigger particle of the dumbbell structure appear almost perfectly hemispherical on the sample surfaces. During heat treatment at lower temperatures mainly the evaporative removal of the big Se particle of the dumbbell structure will take place. Annealing of the smaller particles starts to dominate at temperatures above 240 degrees C and makes the composition of the small particles closer to that of the thermodynamically most favoured In2Se3.     

Chemical synthesis of Cu2Se nanoparticles at room temperature

A simple and rapid method has been developed to synthesize cuprous selenide (Cu₂Se) nanoparticles by the reaction of selenium nanoparticles sol with copper sulfate solution containing ascorbic acid at room temperature. Cu₂Se nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and energy dispersive X-ray analysis (EDX). The results indicated that Cu₂Se nanoparticles were cubic crystal structure and spherical with the diameter about 75 nm. The ultraviolet–visible absorption spectrum (UV–vis) and cyclic voltammetry of Cu₂Se nanoparticles were also investigated. The optical band gap energy of Cu₂Se nanoparticles was 1.94 eV. On the basis of a series of experiments and characterizations, the formation mechanism of Cu₂Se nanoparticles was discussed.     

树枝状与球状PbS纳米结构的组装合成及其形成机理研究

以醋酸铅为铅源,硫代乙酰胺为硫源,在表面活性剂SDS单独作用和表面活性剂SDS和CTAB共同作用下可选择性地组装合成出颗粒以相同晶面粘连组装成的单晶树枝状PbS纳米结构和颗粒以不相同晶面粘连组装成的多晶球状PbS纳米结构,而且提高反应物浓度能起到调节树枝状和球状PbS纳米结构尺寸的作用.对树枝状和球状PbS纳米结构的形成机理进行了初探,发现SDS单独作用时其烷基链起到的软模板作用有利于PbS小颗粒组装成树枝状的PbS纳米结构.当反应溶液中再加入适量的CTAB时,它在溶液中形成微胶束起到了软模板作用,迫使颗粒粘连组装成球状PbS纳米结构,有效地限制树枝状结构的生长.     

Surface-enhanced vibrational spectroscopy of adsorbates on microemulsion synthesized gold nanoparticles

Very small (<10 nm) monodisperse gold nanoparticles (AuNPs) coated with a monolayer of decanethiol were prepared and their surface-enhanced infrared absorption (SEIRA) spectra were measured in the transmission mode. The AuNPs were prepared by the borohydride reduction of HAuCl(4) inside reverse micelles that were made by adding water to a hexane solution of sodium bis(2-ethylhexyl)sulfosuccinate (AOT). The gold nanoparticles were then stabilized by the addition of decanethiol. Subsequent addition of p-nitrothiophenol both facilitated the removal of excess AOT and showed that the gold surface was completely covered by the decanethiol. SEIRA spectra of decanethiol on gold particles prepared in AOT microemulsions were about twelve times more intense than corresponding layers on gold produced by electroless deposition and gave a significantly less noisy spectrum compared to the corresponding surface-enhanced Raman spectrum. The surface-enhanced Raman scattering (SERS) spectra of the same samples showed that the most intense spectrum was obtained from gold nanoparticles with a mean diameter of 2.5 nm. This result is in contrast to previous statements that SERS spectra could only be obtained from particles larger than 10 nm.     

Effect of sodium dodecylsulfate and dodecyltrimethyl ammonium bromide on the morphologies of gold nanoparticles in the presence of poly(amidoamine) dendrimers

The synthesis of gold nanoparticles has been carried out in aqueous phase in the presence of both ionic surfactants (i.e., sodium dodecylsulfate (SDS) and dodecyltrimethylammonium bromide (DTAB)) and poly(amidoamine) dendrimers (PAMAM). It has been observed that the fluoroderivative of 2G PAMAM (2D) acts as reducing agent in reducing Au(lll) to Au(0) leading to the formation of fine gold nanoparticles. This process has been further evaluated in the presence of fixed amounts of both SDS and DTAB in their respective pre and post micellar concentration regions. The presence of SDS leads to the appearance of clear ordered morphologies such as triangular, hexagonal, spherical, and rod shaped, while the presence of DTAB does not show this effect. The formation of nanoparticles in triangular morphologies is more significant in the premicellar concentration range of SDS whereas hexagonal morphologies in the post micellar concentration range. On the contrary, increase in the DTAB concentration from pre to post micellar range only reduces the size of gold nanoparticles without the appearance of any ordered morphology. The formation of ordered gold nanoparticles in the presence of SDS has been further attributed to the significant SDS-dendrimer interactions and an appropriate mechanism has been proposed to justify the results.     

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 and thermal stability of selenium-doped hydroxyapatite with different substitutions

Selenium (Se) plays a specific role in human health, especially for its anti-tumor effect. Incorporation of selenium into biocompatible hydroxyapatite (HAP) may endow the materials with novel characteristics. In the current work, a series of selenium-doped hydroxyapatite (Se-HAP) nanoparticles with different Se/P ratios were synthesized by a modified chemical precipitation. It was revealed that the powders with/without heat-treatment were nano-sized needle-like HAP while the heat-treated samples have high crystallinity. The addition of selenium decreases the crystallinity of the synthesized apatite, and also takes a negative effect on the thermal stability of the as-prepared powders. The Se-HAP nanoparticles with Se/P molar ratio not more than 5% sintered at 900°C can achieve good crystallinity and thermal stability.     

Synthesis and characterization of monodisperse hematite nanoparticles modified by surfactants via hydrothermal approach

Monodisperse rhombohedral α-Fe₂O₃ nanoparticles modified by four different surfactants, sodium dodecylsulfonate (SDS), sodium dodecylebenzene sulphonate (DBS), cetyltrimethyl ammonium bromide (CTAB) and hexadecyipyridinium chloride (HPC), have been synthesized via hydrothermal method, using FeC₂O₄ and NaOH as starting precursors. Meanwhile, monodisperse rodlike α-Fe₂O₃ nanoparticles without surfactant are also prepared under the same conditions for comparison. The products were characterized by means of Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron micrograph (TEM) and magnetization measurements. The products with and without surfactant all exhibit weak ferromagnetic properties at room temperature, except somewhat variation in coercivity values. The experimental results suggest that the surfactants can significantly influence the size and shape of the particles, but cannot affect their magnetic nature.     

纳米粒子对表面活性剂乳液稳定性的影响

制备了由三种不同类型的表面活性剂稳定的乳状液,考察了纳米粒子对表面活性剂乳液稳定性的影响作用,结果表明,ZnO纳米粒子SDBS、Oπ-10和CTAB稳定的乳液均具有破乳作用;MgO纳米粒子对SDBS稳定的乳液具有破乳作用;Fe2O3纳米粒子对三种表面活性剂乳液的稳定性没有显著影响。     

Influence of CTAB surfactant on structural and optical properties of CuS and CdS nanoparticles by hydrothermal route

Metal sulphide CuS and CdS nanoparticles capped with Cetyltrimethylammonium bromide (CTAB) were synthesized by hydrothermal method. Structural, morphological, chemical composition, optical and luminescent properties were evaluated by different analytical techniques. X-ray diffraction (XRD) analysis of the CTAB capped metal sulfide nanoparticles reveals the formation of hexagonal structure. High-resolution transmission electron microscopy (HRTEM) images show that the morphology of the capped copper sulphide samples consists of hexagonal structure and capped cadmium has spherical shape and also confirms the crystalline nature of the particles with distinct lattice fringes. In FTIR spectroscopy, the composition of the CTAB capped CuS and CdS nanoparticles have been confirmed. The analysis of photoluminescence (PL) and optical transition show a red shift due to the reduction of band gap energy and it is attributed to the low defects and high crystallinity. The optical studies indicate that CuS and CdS nanoparticles with CTAB can be suitable for optoelectronic devices and photovoltaic applications.     

Selenium nanowires and nanotubes synthesized via a facile template-free solution method

Trigonal selenium (t-Se) nanowires and nanotubes were successfully prepared on a large scale via an environment-friendly synthetic process, in which no templates or surfactants were employed. These t-Se nanowires having a width of 70-100 nm and length up to tens of micrometers were synthesized in absolute ethanol at room temperature, while t-Se nanotubes with outer diameter ranging from 180 to 350 nm were obtained at 85 °C in water system. SEM and TEM analyses of the samples obtained at different stages indicated that the formation of these t-Se 1D nanostructures was governed by a “solid-solution-solid” growth process. The amorphous Se (a-Se) nanoparticles were initially generated and then would transform into crystal seeds for the subsequent growth of nanowires or nanotubes. Detailed experiments found that temperature and solvents as well as concentrations of starting materials were crucial to the formation of final morphology.     

Pulse and direct electrodeposition of Ni–Co/micro and nanosized SiO2 particles

Ni–Co/SiO₂ composite coating was electrodeposited on the steel substrate. The coatings were characterized by X-ray diffraction and scanning electron microscopy. The microhardness of the composite coatings was studied by variation of the electroplating parameters, such as the pulse current (PC) and direct current (DC) electrodeposition methods, deposition temperature, electrolyte pH, concentration of surfactants, sodium dodecyl sulfate (SDS), and cetyltrimethylammonium bromide (CTAB). Zeta potential of SiO₂ particles measurements was performed with various pH, SDS, and CTAB concentrations. The data depict that the hardness of Ni–Co/SiO₂ nanocomposite coatings manufactured by PC electrodeposition increases with the increase of bath temperature, pH, SDS, and CTAB concentration up to 50°C, 4.6, 0.3, and 0.2?g/L, respectively. Beyond mentioned optimum values, the microhardness of nanocomposite coating decreases. Using DC method led to reduce the microhardness. Utilizing SiO₂ microparticles instead of SiO₂ nanoparticles for reinforcing resulted in declining the microhardness. The friction coefficient and wear results demonstrated that using PC method and nanosized particles led to reduce the friction coefficient and increase the resistance to wear. Anodic polarization results illustrated that using SiO₂ nanoparticles and PC method to prepare coating caused corrosion resistance of coating in a 3.5?wt% NaCl solution to enhance.     

Covalent and noncovalent functionalisation and solubilisation of nanodiamond

Covalent functionalisation of nanodiamond has been carried out by employing several methods. One of them involves the reaction of acid-treated nanodiamond with thionyl chloride followed by reaction with a long-chain aliphatic amine to produce the amide derivative. The second method involves reaction of acid-treated nanodiamond with an organosilicon or organotin reagent such as hexadecyltrimethoxysilane, dibutyldimethoxytin, and perfluoro-octyltriethoxysilane. The products of covalent functionalisation produce excellent dispersions in CCl₄ and toluene. SiO₂–and SnO₂–covered nanodiamond are obtained by heating the nanodiamond coated with the organosilane and the organotin reagents, respectively. By interaction of nanodiamond with surfactants such as sodium bis(2-ethylhexyl) sulphosuccinate (AOT), Triton X-100 (TX-100), polyvinyl alcohol (PVA), cetyltrimethylammonium bromide (CTAB), and tert-octylphenoxy poly(oxyethylene)ethanol (IGEPAL) gives good dispersions in water, the best dispersion with the lowest surfactant concentration being obtained with IGEPAL.     

Preparation,structural characterisation and release study of novel hybrid microspheres entrapping nanoselenium,produced by green synthesis

The main goal of this study was to synthesise and characterise different formulations based on alginate and alginate/chitosan microspheres containing nanoselenium (nano‐Se) for controlled delivery applications. Nanosize elemental selenium was produced by using probiotic yogurt bacteria (Lactobacillus casei) in a fermentation procedure. The structural and morphological characterisation of the microspheres was performed by Fourier transform infrared (FTIR), X‐ray diffraction (XRD) and scanning electron microscopy (SEM) analysis. FTIR and XRD pattern indicated that was an effective cross‐linking of selenium nanoparticles within the polymeric matrix in both cases. The SEM images reveal that selenium nanoparticles are mainly exposed on the surface of alginate, in contrast to porous structure of alginate/chitosan/nano‐Se, interconnected in a regular network. This architecture type has a considerable importance in the delivery process, as demonstrated by differential pulse voltammetry. Selenium release from both matrices is pH sensitive. Moreover, chitosan blended with alginate minimise the release of encapsulated selenium, in simulated gastric fluid, and prolong the duration of release in intestinal fluid. The overall effect is the enhancement of total percentage release concomitant with the longer duration of action. The authors’ formulation based on alginate/chitosan is a convenient matrix to be used for selenium delivery in duodenum, caecum and colon.Inspec keywords: organic‐inorganic hybrid materials, nanocomposites, blending, filled polymers, nanoparticles, nanofabrication, nanomedicine, biomedical materials, drug delivery systems, microorganisms, biological organs, selenium, polymer blends, fermentation, scanning electron microscopy, X‐ray diffraction, Fourier transform infrared spectra, surface morphology, nanoporous materials, porosity, pH, voltammetry (chemical analysis), encapsulationOther keywords: structural characterisation, hybrid microspheres entrapping nanoselenium, green synthesis, alginate‐chitosan microspheres, controlled delivery applications, nanosize elemental selenium, probiotic yogurt bacteria, Lactobacillus casei, fermentation, scanning electron microscopy, morphological characterisation, SEM, Fourier transform infrared spectra, FTIR, XRD, X‐ray diffraction, selenium nanoparticles, polymeric matrix, porous structure, differential pulse voltammetry, pH, blending, encapsulated selenium, simulated gastric fluid, intestinal fluid, total percentage release concomitant, duodenum, caecum, colon, Se     

Synthesis of β-Ag2Se from organo-selenium precursor and silver nitrate in DMF via simultaneous reduction of selenium and silver salt

Reaction of selenium powder and silver nitrate in aqueous N, N′-dimethylformamide (aq. DMF) leads to formation of silver selenide. Similar reaction with cycloalkeno-1,2,3-selenadiazole, an organic compound of selenium upon thermolysis, also produces silver selenide. It is believed that DMF activates selenium and reduces silver salt via in-situ generated hydrogen ion simultaneously. Slightly broadened X-ray diffraction pattern for pure beta silver selenide (β-Ag₂Se) was observed. Scanning electron microscopy (SEM) indicated that the agglomerated particles could be in the range of about 100 to 200 nm in dimension. EDAX analysis showed non-stoichiometric elemental ratio between silver and selenium. It is found that the weight percent of Ag is slightly higher than Se. However, free amorphous selenium is also detected by XPS analysis when the product is made by use of elemental selenium. Thermal analysis (TGA) revealed a small (4%) weight loss due to the presence of organics or the solvent from the reaction medium.     

Fumed silica/polymer hybrid nanoparticles prepared by redox-initiated graft polymerization in emulsions

Hybrid particles comprising aggregated fumed silica nanoparticles as the core and hydrophobic polymers existing around the nanoparticles were prepared by ‘grafting from’ polymerization in emulsions. The emulsion polymerization employed cetyltrimethylammonium bromide (CTAB) as a cationic surfactant and sodium dodecyl sulfate (SDS) as an anionic surfactant, respectively, to stabilize the emulsion polymerization. The polymerization was initiated by the redox reaction between ceric ion Ce(IV) and the amine groups on the surfaces of aminated fumed silica nanoparticles that were modified by 3-aminopropyltriethoxysilane. Infrared spectroscopy and thermogravimetric analysis demonstrated that both poly(methyl methacrylate) (PMMA) and polystyrene (PS) were successfully grafted onto the fumed silica surface. The type of surfactant greatly affected the grafting ratio, monomer-to-polymer conversion, and morphology of the product. When CTAB was used as the surfactant, both the grafting ratio and monomer-to-polymer conversion were lower than when SDS was used, but transmission electron microscopy and light scattering analysis indicated that most of the resultant particles were sub-100 nm hybrid nanoparticles with a non-spherical shape and particles sizes of 75–90 and 57–85 nm for PMMA and PS-grafted fumed silica, respectively. Whereas, when SDS was used as the surfactant, the particles agglomerated to form large irregular clusters or even networks, possibly due to the electrostatic attractions between SDS and Ce(IV) and/or the aminated fumed silica nanoparticles in aqueous solution.     

CTAB作为钒电池电解液添加剂的研究

通过紫外-可见、扫描电镜、方波伏安、循环伏安、稳定性考察,研究了十六烷基三甲基溴化铵(CTAB)作为钒电池电解液的添加剂对电解液的稳定性和电化学活性的影响,并对其机理进行了探讨.研究结果表明:电解液中CTAB胶束的季铵头部基团与五价钒作用,阻止五价钒的进一步聚合,从而抑制了五价钒的结晶.同时,添加剂在电极和电解液界面上,形成稳定的半球状颗粒,起到胶束催化V(IV)/V(V)氧化还原电对的作用.交流阻抗、充放电测试表明添加CTAB的电解液大大减小电荷传递电阻,使双电层电容增大一倍,提高电解液的电化学反应活性,这与CTAB的胶束催化相吻合.