Pulsed sonoelectrochemical synthesis of size-controlled copper nanoparticles stabilized by poly(N-vinylpyrrolidone)

A novel sonoelectrochemical method for the size-controlled synthesis of spherical copper nanoparticles in an aqueous phase was developed. In this study, poly(N-vinylpyrrolidone) (PVP) was used as the stabilizer for the copper clusters. The copper nanoparticles were characterized by XRD, UV-vis, IR, DLS, TEM, and HRTEM. The PVP was found to greatly promote the formation rate of copper particles and to significantly reduce the copper deposition rate, thereby making monodispersed copper nanoparticles. We could control the particle size by adjusting various parameters such as current density, deposition, temperature, and sonic power, and improve the homogeneity of the copper particles. The results also showed that the transfer rate of PVP-stabilized copper clusters from the cathodic vicinity to the bulk solution played an important role in the preparation of the monodispersed nanoparticles.     

CO-assisted synthesis of finely size-controlled platinum nanoparticles

We present a surfactant-free approach for synthesizing size-dependent carbon supported Pt nanoparticles with mean sizes ranging from 4.8 to 1.7 nm by increasing ratios of CO/Ar. In this work, gas stabilizer exhibits the originality on the design of the supported size-controllable clusters.     

Synthesis of copper sulphide and copper nanoparticles with microemulsion method

The present work is focused on the synthesis of nanocopper and nanocopper sulphide metallic particles. The precise control of size and shape is best achievable with microemulsion technique, with in situ synthesis in microemulsion. The effect of most crucial operating parameter, water-to-surfactant molar ratio (w), on the product specification including size as well as size distribution and morphology were investigated. The variation of size was observed with variation in w for copper sulphide and copper. Product specifications were analyzed using transmission electron microscope imaging, dynamic light scattering with particle size analyzer and absorption spectra using UV-visible spectrophotometer. It was observed that bigger particles were achieved at higher water-to-surfactant ratio. From systematic study of effect of w on the size and size distribution of copper nanoparticles, the optimum value was chosen for preparation of in situ catalyst. As copper on alumina catalyst has wide catalytic applications of commercial importance, alumina was selected as support. A novel deposition method is developed successfully to deposit the copper nanoparticles from microemulsion on the support. Thus prepared catalyst was analyzed with UV-visible spectrophotometer and found to contain characteristic peak of copper at 655 nm, indicating proper copper deposition on support. XRD analysis of copper on alumina catalyst confirmed presence of metallic copper.     

Formation of supported size-controlled nanoparticles of sulfated zirconia

Methods of the preparation of catalysts for alkane skeletal isomerization based on uniform nanoparticles of sulfated zirconia anchored to different supports were investigated. These catalysts were characterized by using the ICP, HRTEM and BET techniques. The activities of the catalysts in the reaction of n-butane isomerization were measured and compared with those of bulk catalysts.     

Synthesis and characterization of copper nanoparticles by reducing agent

Cu nanoparticles were synthesized by solution reduction process successfully. The influence of parameters on the size of Cu nanoparticles was studied and the referential process parameters were obtained. The morphology and structure of the synthesized Cu nanoparticles were characterized by transmission electron microscopy (TEM), powder X-ray diffraction (XRD), QELS data, infrared spectroscopy (IR) and solid state UV. The average size of nanoparticles was found between 15 ± 2 nm.     

Synthesis of metallic copper nanoparticles coated with polypyrrole

This paper describes a method for polypyrrole (PPy) coating of metallic Cu nanoparticles in aqueous solution in atmosphere. Colloid solution of Cu nanoparticles was prepared by reducing Cu ions with the use of hydrazine in an aqueous solution dissolving citric acid and cetyltrimethylammonium bromide as stabilizers. The PPy coating was performed by polymerizing pyrrole with the use of hydrogen peroxide as an initiator in an aqueous colloid solution of the Cu nanoparticles. Ultraviolet–visible extinction measurements, transmission electron microscopy observation, and X-ray diffraction measurements revealed that the metallic Cu nanoparticles with a size of 27.6 ± 11.1 nm were coated with PPy. The obtained PPy-coated Cu particles were chemically stable even in atmosphere.     

Synthesis of copper nanoparticles stabilized by polyoxyethylenesorbitan monooleate

We studied the influence of synthesis parameters and the composition of the reaction mixture on the size and morphology of copper nanoparticles (NPs). Use of a surfactant (polyoxyethylenesorbitan monooleate) is promising for confining NP growth and stabilizing NPs. Concentration ranges of existence were determined for copper NP dispersions stable to aggregation and sedimentation. Scanning electron microscopy and dynamic light scattering were used to show that: the NP size varied from 10 to 65 nm, the average diameter was 25–35 nm, and the shape was spherical. The sizes of copper NP aggregates were determined.     

A synthetic route to size-controlled fcc and fct FePt nanoparticles

We report here a new synthetic route to FePt nanoparticles using a stoichiometric mixture of Na2Fe(CO)4 and Pt(acac)2. The structure of FePt nanoparticles, their size, chemical composition, and magnetic property can be controlled by various synthetic parameters, such as the solvent type, nature, and molar ratio of surfactants and stabilizers, synthesis temperature, and purification process. Partially ordered fct (L10) nanoparticles with room temperature magnetic coercivity can be synthesized directly in tetracosane solution at 389 degrees C. The fcc FePt synthesized in nonadecane can be transformed into the magnetically important fct phase at 430 degrees C without significant particle sintering.     

Functional polythiophene nanoparticles: size-controlled electropolymerization and ion selective response

We have synthesized a thiophene derivative, (4-benzeno-15-crown-5 ether)-thiophene-3-methylene-amine (BTA), which was used as a monomer for electrochemical polymerization on metallic surfaces to prepare functional polymer films. Self-assembly of BTA monomers on Au(111) surfaces promotes ordered polymerization to form polymer nanoparticles or clusters by which the size of the polymer nanoparticles can further be controlled electrochemically. The electropolymerization was monitored in situ by scanning tunneling microscopy to unravel the dynamics of the process and possible mechanisms. These are further supported by calculations using a semiquantative model of polymer clusters and X-ray photoelectron spectroscopy analysis. On the basis of these observations, we have attempted to optimize the construction of BTA polymer based ion selective electrodes. The BTA based polymer films, prepared from both aqueous solution and organic phase on gold electrodes, displayed selective sensitivity to potassium ions with a linear dependence of ion concentration over 4 orders of magnitude.     

Synthesis and characterization of metallic copper nanoparticles via thermal decomposition

Copper oxalate was used as a precursor to prepare metallic copper nanoparticles by thermal decomposition. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and UV–Vis spectroscopy. XRD analysis revealed broad pattern for fcc crystal structure of copper metal. The particle size by use of Debye–Scherrer’s equation was calculated to be about 40 nm.     

Spacer-mediated synthesis of size-controlled gold nanoparticles using geminis as ligands

We report a new methodology for the size-controlled aqueous synthesis of gold nanoparticles using geminis with different spacers as ligands. Geminis possess a unique structure in which two hydrophobic chains and two polar headgroups are combined via a spacer. We herein demonstrate that the spacer can be used as a tool to control particle size when geminis are used as ligands for gold nanoparticles. Varying the spacer length of geminis yields facile control over the size and size distribution of nanoparticles. For the 18-s-18-capped gold nanoparticles, FTIR and TGA experiments indicate that the geminis form bilayers on the surface of gold nanoparticles, which serve as templates that control the formation of nanoparticles. The smallest particles are obtained with a moderate spacer length (s = 8) because in that case the gemini bilayers interdigitate to the fullest degree to reach the maximum chain-chain interaction, thus yielding the most compact coating on the surface of gold nanoparticles. This work provides a new approach to the size control of nanoparticles.     

Morphology and size-controlled synthesis of silver nanoparticles in aqueous surfactant polymer solutions

We have employed a number of reducing and capping agents to obtain Ag(0) metallic nanoparticles of various sizes and morphologies. The size and morphology were tuned by selecting reducing and capping agents. Spherical particles of 15 and 43 nm diameter were obtained when 1 wt% aqueous starch solution of AgNO₃ precursor salt was reduced by d(+)-glucose and NaOH, respectively, on heating at 70 °C for 30 min. Smaller size particles obtained in the case of d(+)-glucose reduction has been attributed to the slow reduction rate by mild reducing agent d(+)-glucose compared to strong NaOH. Conducting the reduction at ambient temperature of silver salt in liquid crystalline pluronic P123 and L64 also gave spherical particles of 8 and 24 nm, respectively, without the addition of any separate reducing agent. NaOH reduction of salt in ethylene glycol (11 g)/polyvinyl pyrolidone (PVP; 0.053 g) mixture produced large self-assembled cubes of 520 nm when smaller (26–53 nm) star-shaped sharp-edged structures formed initially aggregated on heating the preparation at 190 °C for 1 h. Increasing the amount of PVP (0.5 g) in ethylene glycol (11 g) and heating at 70 °C for 30 min yielded a mixture of spherical and non-spherical (cubes, hexagons, pentagons, and triangle) particles without the addition of an extra reducing agent. Addition of 5 wt% PVP to 1 wt% aqueous starched solution resulted in the formation of a mixture of spherical and anisotropic structures when solution heated at 70 °C for 1 h. Homogeneous smaller sized (29 nm) cubes were synthesized by NaOH reduction of AgNO₃ in 12.5 wt% of water-soluble polymer poly(methyl vinyl ether) at ambient temperature in 30 min reaction time.     

Synthesis, characterization, and antifouling potential of functionalized copper nanoparticles

The synthesis, characterization, and antimicrobial properties of functionalized copper nanoparticle/polymer composites are reported. Copper nanoparticles (Cu NPs) are stabilized by surface attachment of the acrylic functionality that can be copolymerized with other acrylic monomers, thus, becoming an integral part of the polymer backbone. Biological experiments show that Cu NP/polymer composites exhibit antimicrobial activity similar to that of conventional copper-based biocides. Atomic absorption spectroscopy shows the smallest amount of copper ions leaching from chemically bound acrylated Cu NPs compared to the nonfunctionalized biocides. These composites have a strong potential for use in antibacterial or marine antifouling coatings.     

Synthesis and size control of monodisperse copper nanoparticles by polyol method

We describe herein the synthesis of metallic copper nanoparticles in the presence of poly(vinylpyrrolidone), employed as a protecting agent, via a polyol method in ambient atmosphere. The obtained copper particles were confirmed by XRD to be crystalline copper with a face-centered cubic (fcc) structure. We observed monodisperse spherical copper nanoparticles with a diameter range 45+/-8 nm. The particle size and its distribution are controlled by varying the synthesis parameters such as the reducing agent concentration, reaction temperature, and precursor injection rate. The precursor injection rate plays an important role in controlling the size of the copper nanoparticles. On the basis of XPS and HRTEM results, we demonstrate that the surface of the copper is surrounded by amorphous CuO and that poly(vinylpyrrolidone) is chemisorbed on the copper surface.     

Pyrene-assisted synthesis of size-controlled gold nanoparticles in sodium dodecyl sulfate micelles

Gold nanoparticles prepared by chemical reduction in sodium dodecyl sulfate (SDS) solution are size-controlled with the addition of pyrene. Micellar electrokinetic capillary chromatography (MEKC) is applied to the system to examine the size and polydispersity of gold nanoparticles and to show that pyrene has the extraordinary effect in decreasing the size and narrowing the dispersity of gold nanoparticles. The MEKC electropherograms further suggest that pyrene could be oxidized by the aqueous Au(III) complexes first. All the reduced Au complexes were then solubilized in the pyrene-SDS micelles. The growth of gold nanoparticles beyond the embryonic stage was subsequently inhibited by the encapsulating SDS and electrophilic pyrene.     

Synthesis of copper nanoparticles in the matrix of ethylene-propylene copolymer

Copper nanoparticles in the matrix of ethylene propylene copolymer were derived by a method of a high thermal decomposition of an organometallic precursor in a high shear. It was revealed that the decomposition temperature of the precursor increases significantly in the formation of nanoparticles in the polymer matrix. It was found by X-ray diffraction analysis and scanning electron microscopy that copper nanoparticles in shape close to spherical and of a wide particle size distribution are formed in the decomposition of copper formate dihydrate in an elastomeric matrix.     

Magnetic nanoparticles supported copper catalysts: Synthesis of heterocyclic scaffolds

Abstract

Heterocyclic scaffolds are important components in the structure of many drugs and natural products. They are well-known compounds because of their broad spectrum of pharmaceutical and biological activities. In this paper, we provide an overview of the utilization of copper complexes immobilized on magnetic nanoparticles as economical and efficient catalytic systems for the synthesis of heterocyclic molecules.     

One-step fabrication of ultralow dielectric polyimide films consisting of size-controlled mesoporous nanoparticles

Dielectric materials with ultralow dielectric constants (<2.0) are desiderated in the integrated circuits (ICs). In this work, we fabricated polyimide (PI) films consisting of mesoporous nanoparticles (MPNPs-PF) through a one-step solvent evaporation induced self-assembly method. Poly(amic acid) was selected as the polymer matrix; and the commercial triblock copolymer F127 was adopted as the mesoporous template as well as the nanoparticle morphology controller, respectively. After imidization and template removal, the dense films consisting of closed-packed PI nanoparticles with an average diameter less than 50 nm were obtained. Since the nanoparticles were fully composed of worm-like mesopores, the dielectric constant (k value) of the resultant porous PI films can reach as low as 1.92. When the reactive end-capper of maleic anhydride (MA) was blended into poly(amic acid), k value decreased even lower to 1.86. Meanwhile, the modulus of the resultant porous PI films was higher than 1 GPa.     

Selective heterogeneous nucleation and growth of size-controlled metal nanoparticles on carbon nanotubes in solution

We present a novel approach to the in situ deposition of size-controlled platinum nanoparticles on the exterior walls of carbon nanotubes (CNTs). The reduction of metal ions in ethylene glycol (EG), by the addition of a salt such as sodium dodecyl sulfate (SDS), p-CH3C6H4SO3Na, LiCF3SO3, or LiClO4, results in high dispersions and high loadings of platinum nanoparticles on CNTs without aggregation. We have performed controlled experiments to elucidate the mechanism. By exploiting the salt effect, our method effectively depresses homogeneous nucleation, leading to selective heterogeneous metal nucleation and growth, even on unmodified CNTs. In the 2.3-9.6 nm size range, the size of platinum nanoparticles, at 50% loading, can be controlled by changing the concentration of metal ions, the reaction temperature, the reducing reagent or the means by which reactive solutions are added. Our method provides a flexible route towards the preparation of novel one-dimensional hybrid materials, for which a number of promising applications in a variety of fields can be envisioned.