Preparation and characterization of gold nanoparticles using ascorbic acid as reducing agent in reverse micelles

In this study, well-dispersed gold nanoparticles were prepared by the reduction of HAuCl₄ in sodium bis(2-ethylhexyl)sulfosuccinate/isooctane reverse micelles system using ascorbic acid as reducing agent. The properties of the obtained nanoparticles were characterized with transmission electron microscopy, X-ray diffraction, thermogravimetric analysis, and UV–vis absorption spectrophotometer. Due to its high water solubility, biodegradability, and low toxicity, ascorbic acid could be used as a benign naturally available reducing agent to synthesize gold nanoparticles.     

Synthesis and magnetic properties of Fe3O4 nanoparticles

Ferromagnetic Fe₃O₄ nanoparticles with diameter of ∼27 nm were prepared by a hydrothermal route in the presence of a surfactant, sodium bis(2-ethylhexyl)sulfosuccinate (AOT). The as-synthesized product was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The hysteresis loops of the iron oxide nanoparticles were measured using a physical property measuring system (PPMS), and the results showed a superparamagnetic behavior at room temperature.     

Synthesis,size control,and passivation of CdS nanoparticles in water/AOT/n-heptane microemulsions

CdS nanoparticles have been synthesised by adding tetrabutylammonium hydrogen sulphide to water/sodium bis(2-ethylhexyl) sulfosuccinate/n-heptane microemulsions containing CdSO₄. Analysis of UV–Vis absorption spectra recorded at various times indicates that an initial rapid formation of CdS nanoparticles is followed by a very slow growth process which can be well described by a power law. The growth process is totally inhibited by the addition of an appropriate amount of bis(2-ethylhexyl)amine (BEA) leading to the formation of stable nanosized CdS particles coated by an oriented monolayer of chemically bonded BEA molecules. Depending on the BEA addition time, the growth inhibition can be achieved at any moment of the process leading to an easy and fine size control. The main advantage of this procedure is that the BEA-coated CdS nanoparticles can be easily separated from the reaction medium and dispersed in nonpolar media such as heptane and in polar media such as an aqueous surfactant solution.     

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.     

Porous polypyrrole/polymethylmethacrylate composite film prepared by vapor deposition polymerization of pyrrole and its application for ammonia detection

A simple method has been developed to fabricate porous polypyrrole/polymethyl methacrylate composite films. The synthesis procedures include the vapor deposition polymerization of pyrrole on the composite films of polymethyl methacrylate and ferric hydroxide bis(1,4-bis(2-ethylhexyl) sulfosuccinate), successively, washing the obtained composite films with methanol. Scanning electron microscopic and microscopic Raman spectral studies indicated that the pores had an average size of about 5 μm and they were uniformly dispersed in the whole films. The electrical conductivities of the composite films were measured to be in the range of 10^− 3 to 10^− 2 S cm^− 1. The porous composite films showed electroactivity, and the sensors based on them exhibited high sensitivity and fast response to ammonia gas.     

Characterization of mono- and multilayered films with Mn-doped ZnS nanoparticles and luminescence properties of the monolayered films prepared by applying magnetic fields

Mn²⁺-doped ZnS (ZnS:Mn) nanoparticles were prepared using bis(2-ethylhexyl) sulfosuccinate (AOT) reversed micelle method. Luminescence at 583-589 nm were observed in the ZnS:Mn nanoparticles and are ascribed to Mn²⁺ ion in the nanoparticles due to energy transfer from ZnS. The luminescence was enhanced by capping with alkanethiol. Mono-and multilayered films with the alkanethiol-capped ZnS:Mn nanoparticles were fabricated on quartz substrates by layer-by-layer method using self-assembled monolayer (SAM) of 1,6-hexanedithiol. The polarization degrees of luminescence for the monolayered films were enhanced by preparation under applying magnetic field. The enhancements are probably caused by magnetic orientation of the ZnS:Mn nanoparticles on the quartz substrates.     

Conducting polymer coated graphene oxide reinforced C–epoxy composites for enhanced electrical conduction

Enhanced electrical conductivities were achieved in C–epoxy composites by integrating them with conducting polymers (CPs), namely poly pyrrole (PPY), poly(3,4-ethylene dioxythiophene) (PEDOT) and graphene oxide (GO) enwrapped by CPs. By in-situ polymerization of pyrrole or 3,4-ethylenedioxythiophene (EDOT) in the presence of the GO (template), sodium bis(2-ethylhexyl) sulfosuccinate (structure directing agent), ferric chloride (oxidant), the electrically conductive sheets of GO enwrapped CPs were obtained. The formation of CP coating on GO was confirmed by Raman spectroscopy, scanning electron microscopy and thermo gravimetric analysis studies. Different wt% of CP and CP coated GO were added to the epoxy resin and this resin was used to prepare the 2D laminated C–epoxy composites by hand layup method. DC electrical conductivity of the prepared C–epoxy composites were analyzed using current–voltage (I–V) characteristics and impedance measurements. Typical results showed that CP coated GO, at 0.5 wt% addition to epoxy imparted highest DC electrical conductivity for C–epoxy composite.     

Synthesis of Ni nanoparticles by reduction of NiCl2 ionic clusters in the confined space of AOT reversed micelles

Stable Nickel nanoparticles have been synthesized by a novel synthetic route based on the reduction of NiCl₂ ionic clusters in the confined space of reversed micelles. The reaction was carried out by adding anhydrous NaBH₄/ethanol solution to a solution of NiCl₂ ionic clusters nanoencapsulated in bis(2-ethylhexyl)sulfosuccinate (AOT) reversed micelles in the presence of n-dodecylmercaptane as capping agent. As highlighted by FT-IR, an extraction with water eliminates surfactant and side products leaving lipophilic Nickel nanoparticles to be dispersed in the organic solvent. UV-Vis investigation ascertained the formation of stable metal Nickel nanoparticles exhibiting novel optical properties.     

Size-controlled synthesis of ZrO2-TiO2 nanoparticles prepared via reverse micelle method: Investigation of particle size effect on the catalytic performance in vapor phase Beckmann rearrangement

Zirconium-titanium mixed oxide nanoparticles have been synthesized using microreactors made of bis-(2-ethylhexyl) sulfosuccinate (AOT)/water/n-hexane microemulsions. The control of particle size was achieved by varying the process variables, such as water-to-surfactant molar ratio and reagent concentration. Their sizes, appearances, crystal structures, pore diameter and surface area were characterized by TEM, XRD, N₂ adsorption/desorption methods. The results revealed that samples prepared in reverse micelles had no crystalline phase. The Beckmann rearrangement of cyclohexanone oxime on ZrO₂-TiO₂ nanoparticles was carried out in a fixed-bed down flow reactor to investigate the effect of particle size on catalytic activity and selectivity. Samples synthesized in reverse micelles had better reaction performance than samples prepared via sol-gel method. A parallel relationship could be drawn between the catalytic activity and the particle size as well as the selectivity of the catalyst.     

Synthesis, characterization, and antibacterial activity of silver-doped silica nanocomposite particles

Silver nanoparticles were adsorbed preferentially on silica surface to form composite particles using a reverse micelle process that stabilizes the silver particles by an anionic sodium bis(2-ethylhexyl) sulfosuccinate (AOT) surfactant in isooctane solvent together with the silica particles in which their surface being mediated by a cationic poly(allylamine hydrochloride) (PAH) polyelectrolyte. The heterogeneous adsorption was rendered by both electrostatic attraction and hydrophilic/hydrophobic interaction, and was carried out in multiple deposition cycles. The resulting nanocomposite particles were characterized by zeta-potential measurement, electron microscopy, X-ray diffractometry, field-emission electron spectroscopy for chemical analysis (ESCA), and inductively coupled plasma analysis, respectively. In addition, antibacterial activity of the composite particles was examined against Escherichia coli (E. coli) in aqueous environment.     

Calorimetric study of CdS nanoparticle formation in w/o microemulsions

The formation of CdS nanocrystals in ternary w/o microemulsions of sodium bis(2-ethylhexyl) solfosuccinate/water/isooctane and in quaternary w/o microemulsions of cetyltrimethylammonium bromide (CTAB)/n-pentanol/water/n-hexane was studied by calorimetric measurements. In order to gain information on the role played by the various factors governing the formation of nanoparticles, the enthalpy of formation of CdS nanocrystals in microemulsion was investigated as a function of W₀, the molar ratio between water and surfactant and P₀, the molar ratio between alcohol and surfactant. Different energetic states of CdS nanocrystals in microemulsions and in water and a dependence of them on the composition and nature of the microemulsive system are evidenced.     

Chemical synthesis and low temperature electrical transport in polypyrrole doped with sodium bis(2-ethylhexyl) sulfosuccinate

Polypyrrole (PPy) is polymerized by chemical oxidative polymerization in presence of anionic surfactant sodium bis (2-ethylhexyl) sulfosuccinate (DEHS) as the dopant. The electrical conductivity was optimized in terms of oxidant to monomer molar ratio and polymerization yield was measured for these reactions. We have used ammonium persulphate (APS) as the oxidant for polymerization in this series of experiments. The effect of concentration of oxidant on the electrical conductivity is examined. Chemical synthesis of polypyrrole is supported by FTIR spectrum. The electrical conductivity of doped and undoped polypyrrole has been measured in the temperature range of 10–300 K and is found to increase with rise in temperature. Electrical conductivity of PPy was analyzed in the light of various charge transport models. Analysis of the electrical conductivity data reveals that in the temperature range 60–300 K electrical transport is predominantly governed by power law behaviour given by Kivelson model. However in the low temperature range 10–60 K electrical transport is dominated by the fluctuation assisted mechanism.     

Mechanical alloying and sintering of nanostructured tungsten carbide-reinforced copper composite and its characterization

Elemental powders of copper (Cu), tungsten (W) and graphite (C) were mechanically alloyed in a planetary ball mill with different milling durations (0–60 h), compacted and sintered in order to precipitate hard tungsten carbide particles into a copper matrix. Both powder and sintered composite were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) and assessed for hardness and electrical conductivity to investigate the effects of milling time on formation of nanostructured Cu–WC composite and its properties. No carbide peak was detected in the powder mixtures after milling. Carbide WC and W₂C phases were precipitated only in the sintered composite. The formation of WC began with longer milling times, after W₂C formation. Prolonged milling time decreased the crystallite size as well as the internal strain of Cu. Hardness of the composite was enhanced but electrical conductivity reduced with increasing milling time.     

聚乙烯醇-聚吡咯复合纳米纤维的制备及其导电性能

利用化学氧化法制备出导电聚吡咯（PPy）,与聚乙烯醇（PVA）共混后,采用静电纺丝技术制备PVA-PPy纳米共混纤维,随后加入对甲苯磺酸钠（TSNa）、十二烷基磺酸钠（DSNa）、十二烷基苯磺酸钠（DBSNa）和磺基琥珀酸二乙基己酯钠（DEHS）等不同掺杂剂改变纤维的结构和性能,采用SEM、TGA和四探针测试仪检测了纳米纤维的形貌、热稳定性和导电性能。结果表明,掺杂剂、PPy制备技术及聚合物添加剂对PPy的形貌、热稳定性和导电性能有很大影响。纳米纤维的电导率远远高于用同样掺杂剂所制备的PVA-PPy薄膜和PPy粉末,四种纳米纤维中DEHS掺杂PVA-PPy纳米纤维的电导率最高,可达26.64 S/cm。     

A method for synthesizing the core (Ag)/shell (PSt) composite nanoparticles

Core-shell composite materials have been widely used in many fields. In this paper, the core (Ag)-shell (PSt) composite nanoparticles have been successfully fabricated in microemulsions at ambient pressure. Firstly, Ag nanoparticles with about 60-100 nm in diameters were synthesized by reducing silver nitrate by ascorbic acid, and then, styrene polymerized at the surface of Ag nanoparticles by K₂S₂O₄ initiator in microemulsion solutions. The Ag/PSt core-shell composite nanoparticles were identified by transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and infrared spectra (IR). Results show that Ag-core nanoparticles were coated with ultra thin PSt shell with thickness of about 3-6 nm.     

Deuterium post-metallization anneal of electrochemical-plated Cu film deposited on different barrier materials

In this paper, we report on electrochemical-plated (ECP) copper (Cu) film characterizations with different (Ta, TaN and TiN) barrier materials subjected to post-metallization-annealing (PMA) in deuterium (D₂) under various annealing conditions. For comparison, post-metallization-anneal of the ECP Cu film in pure nitrogen (N₂) and forming gas (20% hydrogen+80% nitrogen) were also performed. We used four-point probe to determine the sheet resistance. Scanning electron microscopy was used to examine the surface morphology of the after-annealed ECP Cu films. X-ray-diffraction (XRD) analysis was used to inspect the texture of the ECP Cu films before and after PMA. The deuterium distribution in the barrier layer was determined by using the secondary ion mass spectroscopy depth profile analysis. We found that under appropriate PMA conditions, the sheet resistance of ECP Cu films deposited on TaN barrier was the lowest after D₂ PMA when compared with those deposited on TiN and Ta barriers.     

Characterization of conductive composite films based on TEMPO-oxidized cellulose nanofibers and polypyrrole

Abstract  

In this article, conductive composite films based on TEMPO-oxidized cellulose nanofibers (TOCN) and polypyrrole (PPy) were synthesized in situ by a Chemical Polymerization Induced Adsorption Process of pyrrole on the surface of TOCN in aqueous medium. Resulting composite films were investigated by X-ray photoelectron spectroscopy, scanning, and transmission electron microscopy, N₂ gas adsorption analysis, thermogravimetric analysis, mechanical tests, and conductivity measurements in the ambient air. Our results showed a stable, flexible, and highly electrically conductive composite film in which PPy nanoparticles coated the surface of the TOCN network. In addition, the advantage in using the famous material, TOCN, is clearly due to the presence of carboxylate (COOH/COO⁻Na⁺) and hydroxyl (OH) moieties on the surface of TOCN. These reactive moieties could enhance the adsorption process of positively charged PPy backbone during polymerization. TEM observations demonstrated the formation of a PPy coat along the surface of the cellulose nanofibers having a diameter of about 90 nm which is relatively higher compared to the initial diameter of pure TOCN (~9 nm). Despite the physical and chemical treatment of TOCN during polymerization, the micrometric length of the cellulosic nanomaterial was maintained. In addition, the incorporation of polyvinyl alcohol as an additive in the TOCN/PPy composite seems to enhance the flexibility of composite films (bent up to 180°) without losing the high electrical conductivity. Finally, because of the high conductivity and good mechanical properties of the TOCN/PPy composite films obtained in this work, they can be used as a promising material in applications of sensors, flexible electrodes, and other fields requiring electrically conductive flexible films.     

Thin films of molybdenum and tungsten disulphides by metal organic chemical vapour deposition

Thin films of MoS₂ and WS₂ have been prepared on various substrates (glass, quartz, LiF, MgO, mica, molybdenum, gold, platinum, aluminium, copper, steel, graphite, MoSe₂) by metal-organic chemical vapour deposition using sulphur or hydrogen sulphide and the hexacarbonyls of the transition metals as volatile components. The deposition technique is described here. The thin layers have been examined by X-ray powder diffraction and scanning electron microscopy. Time-resolved microwave conductivity measurements were used to detect the photoactivity of these materials.     

Microstructure and electrical properties of RuO2-CeO2 composite thin films

RuO₂-CeO₂ composite thin films are deposited on various Si substrates by a radiofrequency magnetron sputtering technique. Compacted polycrystalline pellets of the nanostructured CeO₂-RuO₂ composite system are used as standard samples for comparative electrical analyses. All films and composite samples are analyzed by X-ray diffraction and transmission electron microscopy. Electrical measurements of radiofrequency sputtering of thin films are performed as a function of the RuO₂ fraction and of the temperature (between 25 and 400 °C). A nonlinear variation in the electrical conductivity of the RuO₂-CeO₂ composite thin films as a function of the RuO₂ volume fraction (Φ) is observed and discussed. It is interpreted in terms of a power law (in (Φ − Φc)^m ), where m and Φc are parameters characteristic of the distribution of the conducting phase in a composite medium.     

Polyaniline–CuO hybrid nanocomposites: synthesis, structural, morphological, optical and electrical transport studies

Thin films of semiconducting polyaniline (PANi) nanofibers reinforced with copper oxide (CuO) nanoparticles (NPs) were prepared on glass substrate using spin coating technique. Polyaniline (PANi) have been synthesized by chemical oxidative polymerization method with monomer aniline in presence of (NH₄)₂S₂O₈ as an oxidant at 0 °C. The copper oxide (CuO) nanoparticles were synthesized by sol–gel method. Physical properties of nanocomposite (NCs) films were characterized and analyzed by X-ray diffraction, Scanning electron microscopy, Fourier transform infrared (FTIR) spectroscopy, UV–vis spectroscopy, Two probe resistivity measurement technique and Thermo-emf measurement. Structural analysis showed that the crystal structure of CuO is not disturbed in the PANi–CuO hybrid nanocomposite. Surface morphology study shows the uniform distribution of CuO nanoparticles in PANi matrix. FTIR and UV–Visible studies confirm the presence of polyaniline in emeraldine base form in the composites and suggest incorporation of CuO in polymer. Two probe electrical resistivity measurements of nanocomposites (NCs) film revealed that the resistivity of PANi increases with increasing content of CuO NPs.