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.     

Photocatalytic mineralization of carboxylic acids over Fe-loaded ZnS nanoparticles

Zinc sulfide (ZnS) nanoparticles prepared by hydrothermal synthesis were subsequentially impregnated with different iron amounts (0.5−5.0 at%) to obtain Fe-loaded ZnS nanoparticles. Phase composition, crystallinity, crystal size, and morphology of 0.5–5.0 at% Fe-loaded ZnS nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDXS), X-ray photoelectron spectroscopy (XPS), and inductively coupled plasma (ICP). Specific surface area determined by the Brunauer, Emmett and Teller (BET) method was found to be in the range of 85–197 m²/g. The average particle size obtained from TEM analysis of pure ZnS and 2.0 at% Fe-loaded ZnS nanoparticles was 5–20 nm. The optical absorption properties of the samples measured by UV–vis diffuse reflectance spectroscopy (UV–vis DRS) clearly indicated the bathochromic shift upon loading ZnS with Fe. Photocatalytic activities of pure ZnS and Fe-loaded ZnS nanoparticles were examined by studying the mineralization of oxalic acid and formic acid under UVA illumination. It was found that 2.0 at% Fe-loaded ZnS sample exhibited the highest degradation activity possibly due to the presence of Fe in an optimum amount and the increases of surface area and light absorption in UVA region.     

Synthesis of copper nanoparticles by electrolysis of DNA utilizing copper as sacrificial anode

Copper nanoparticles have been synthesized by anodic oxidation through a simple electrolysis process employing de-oxy ribonucleic acid (DNA) as electrolyte. Platinum was taken as cathode and copper as anode. The applied voltage was 4 V and the electrolysis was performed for duration of 1 h. The copper nanoparticles were prepared in situ from the electron beam irradiation on residues of electrolyte consisting of DNA and copper particles: DNA (Cu) complexes. The size of the nanoparticles ranges between 5-50 nm. A tentative explanation has been given for the formation of copper nanoparticles.     

Synthesis of copper nanoparticles using soybeans as a chelant agent

The preparation of stable, uniform copper nanoparticles by the formation of a complex Cu-soybeans extract and the reduction by sodium borohydride are reported in the present paper. It is a simple process for obtaining copper nanoparticles. The samples have been characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM), which reveal the nature of the nanoparticles. These studies reveal that the particles are mostly spherical in shape and have an average size of 20 nm. The UV-vis spectra show that an absorption band, occurring because of Surface Plasmon Resonance, exists at 545 nm; the size distribution is measured with DLS.     

Synthesis of copper ferrite nanoparticles

Pseudospherical copper ferrite particles 20 to 90 nm in average size were prepared by an aerosol method through condensation of iron and copper vapors in an inert-gas flow, followed by the oxidation of the resulting two-phase powder under heterogeneous combustion conditions to an almost single-phase product. The nanoparticles were characterized by scanning electron microscopy, X-ray diffraction, BET measurements, and vibrating-sample magnetometry. Analysis of the X-ray diffraction data and the behavior of the magnetization of reaction intermediates and final synthesis products in the range 400–1100 K made it possible to propose models for the nanostructure of the particles and establish the likely sequence of the observed phase transformations.     

Synthesis and characterization of bismuth doped barium sulphide nanoparticles

We have synthesized BaS:Bi nanocrystalline powder of average grain size 35 nm by solid-state diffusion method using sodium thiosulphate as a flux. During this work we have optimized the nature and amount of flux, amount of the dopant and temperature of firing for maximum yield of photoluminescence. The samples were characterized by X-ray powder diffraction (XRD) method, transmission electron microscopy (TEM), photoluminescence (PL) and UV-visible techniques. On excitation by 425 nm, these nanophosphors give one emission peak at 575 nm which corresponds to green color. In the excitation spectra of these particles there are two peaks at 350 nm and 425 nm. The effect of dopant concentration on the photoluminescence of BaS:Bi nanocrystallites has been studied which is in agreement with the principle of concentration quenching. The energy band gap of bismuth doped BaS nanopowder has been calculated to be 4.25 eV and is blue shifted in comparison to their bulk counterparts. The blue shift may be due to the quantum confinement in the particles.     

Synthesis and characterization of copper nanoparticles

Reduction of copper salt by sodium citrate/SFS and myristic acid/SFS leads to phase pure Cu nanoparticles. However, a similar reaction with hydrazine hydrate (HH) and sodium formaldehyde sulfoxylate (SFS) in polymer afforded only a mixture of Cu₂O and Cu. Copper nanoparticles so-prepared were characterized by UV-Visible spectroscopy, X-ray diffraction measurements (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Freshly prepared solutions showed an absorption band at about 600 nm due to surface plasmon resonance (SPR). XRD analysis revealed all relevant Bragg's reflection for fcc crystal structure of copper metal. The particle size by use of Scherrer's equation is calculated to be about 30 nm. TEM showed nearly uniform distribution of the particles in PVA.     

Synthesis of copper nanoparticles in polycarbonate by ion implantation

Copper nanoparticles have been synthesized in polycarbonate by 75 KeV Cu⁻ ion implantation with various doses ranging from 6.4 × 10¹⁵ to 1.6 × 10¹⁷ ions/cm² with a beam current density of 800 nA/cm². The composites formed were structurally characterized using Ultraviolet-Visible (UV-Visible) absorption spectroscopy. The appearance of particle plasmon resonance peak, characteristic of copper nanoparticles at 603 nm in absorption spectra of polycarbonate implanted to a dose of 1.6 × 10¹⁷ ions/cm², indicates towards the formation of copper nanoparticles in polycarbonate. Transmission electron microscopy further confirms the formation of copper nanoparticles having size ∼ 3.15 nm. The formation of copper nanoparticles in the layers carbonized by Cu⁻ implantation has been discussed. The synthesized copper-polycarbonate nanocomposite has been found to be more conducting than polycarbonate as ascertained using current-voltage characteristics.     

Synthesis of copper nanoparticles by solid-state plasma-induced dewetting

Copper nanoparticles were prepared by the plasma treatment of Cu thin films without extra heating. The Cu nanoparticles were formed through a solid-state dewetting process at temperatures of less than 450 K. The particle sizes, from 10 to 80 nm, were controlled by changing the thickness of the Cu film; the particle size increased linearly with the film thickness. The Cu nanoparticles produced by plasma treatment showed an excellent size uniformity compared to those prepared by heat treatment. In the early stage of the dewetting of the Cu film, uniformly distributed holes nucleated, and the holes grew and coalesced until the Cu nanoparticles were formed. The low operating temperatures used contributed to the production of uniform Cu nanoparticles.     

Synthesis of copper indium sulfide nanoparticles by solvothermal method

Single crystalline CuInS₂ particles with a chalcopyrite structure and a size of 7–10 nm were prepared by a convenient solvothermal reaction, and characterized by XRD, XPS, TEM (HR-TEM) and UV–vis absorption spectroscopy. The as-synthesized nanoparticles can be redispersed in organic solvents, which will facilitate the practical application of these nanoparticles under organic-solution conditions. The growth of the CuInS₂ is regarded to involve the formation and decomposition of Cu²⁺-thiourea complexes, the reduction of Cu²⁺ and a slow supply of In³⁺ ions in the crystallization solution.     

Properties of zinc sulphide nanoparticles stabilized in silica

Zinc sulphide nanoparticles have been synthesized in silica matrix using sol-gel method. It is observed that silica could be loaded with zinc sulphide over a very wide range of concentration without changing the nanoparticle size. A strongly luminescent zinc sulphide-silica composite, thermally stable even upto 700°C was thus obtained. Several techniques like UV absorption, photoluminescence, x-ray diffraction, scanning electron microscopy, transmission electron microscopy, thermogravimetry and photoelectron spectroscopy have been performed to analyse the ZnS-silica composites.     

Simple new synthesis of copper nanoparticles in water/acetonitrile mixed solvent and their characterization

Copper nanoparticles were successfully synthesized by the borohydride reduction of copper nitrate salt in water/CH₃CN mixed solvent under inert argon-purged conditions. Cu nanoparticles were synthesized in large-scale production for the first time by introducing CH₃CN into water and preventing oxidation during the preparation of nanoparticles. Nanoparticles were characterized by using UV-visible absorption spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) techniques. High resolution TEM pictures showed the formation of homogeneous cubic-structured copper nanoparticles with sizes less than 100 nm. This new kind of synthesis method shows the excellent stability compared with that of citrate-protected copper nanoparticles, which may provide an efficient way to improve the fine tuning of the structure and size of copper nanoparticles.     

Synthesis and properties of a water-soluble ionic conjugated polymer with carboxylic acids

A new water-soluble ionic conjugated polymer, poly[N-(carboxymethyl)-2-ethynylpyridinium bromide], was prepared by the activated polymerization of 2-ethynylpyridine by using bromoacetic acid. This polymerization proceeded well in mild reaction conditions without any additional initiator or catalyst. The polymer structure was characterized by various instrumental methods to have a conjugated polymer backbone system with the designed functional groups. The photoluminescence spectrum of polymer showed that the PL peak is located at 603 nm corresponding to the photon energy of 2.06 eV. The cyclovoltammograms of polymer exhibited the irreversible electrochemical behaviors between the oxidation and reduction peaks. The oxidation current density of polymer versus the scan rates is approximately linear relationship in the range of 30 mV/sec-150 mV/sec. It was found that the kinetics of the redox process of polymer is almost controlled by the reactant diffusion process from the oxidation current density of polymer versus the scan rates.     

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.     

Spectroscopic and electrochemical studies on the molecular interaction between copper sulphide nanoparticles and bovine serum albumin

The interaction of covellite hexagonal phase of copper sulphide nanoparticles (CuS NPs) with bovine serum albumin (BSA) was examined systematically by using fluorescence, UV–visible, circular dichroism (CD), Fourier transform infrared (FTIR), dynamic light scattering (DLS) and molecular modelling techniques. Electrochemical method was studied to further confirm the interaction of BSA with CuS NPs. The results of fluorescence studies demonstrated that fluorescence of BSA was quenched by CuS NPs via a static quenching mechanism. The negative values of thermodynamic parameters (ΔG, ΔH and ΔS) indicated that the binding process is spontaneous, exothermic and van der Waals force or hydrogen bonding plays major roles in the interaction of CuS NPs with BSA. The interaction of CuS NPs with Trp residue was established by synchronous studies, and competitive binding studies revealed that Trp-212 of subdomain IIA was involved in the interaction with these nanoparticles. Further, the efficiency of energy transferred and the distance between fluorophore (BSA) and acceptor (CuS NPs) were calculated using Forster’s resonance energy transfer theory. The results of UV–visible, CD, FTIR and DLS revealed that the CuS NPs interact with BSA by inducing the conformational changes in secondary structure and reducing the α-helix content of BSA. Molecular modelling studies suggested that CuS NPs bind to site I of sub domain IIA of BSA. The results of spectroscopic and molecular docking studies were complimented by the electrochemical techniques.     

Laser synthesized TiO2-based nanoparticles and their efficiency in the photocatalytic degradation of linear carboxylic acids

Abstract

Titanium dioxide nanoparticles were synthesized by laser pyrolysis, their surface and electronic properties were modified by gold and/or nitrogen. These materials were characterized by different techniques like X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance (EPR). Time resolved conductivity (TRMC) was used to study the charge separation of electron/hole pairs. Altogether (XPS, EPR, TRMC), the physicochemical characterizations are well correlated with chemical photoactivity of the different samples. Their photocatalytic activity was evaluated for the degradation of linear carboxylic acids (C2-C3) under UV and visible illumination. The decomposition rate of acids was measured, it shows that the modification with gold increases the photoactivity while the presence of nitrogen slows down the process. Such observations are in good agreement with evolution of TRMC signals. A degradation pathway has been determined by identification of intermediate products by chromatography and EPR, results show different intermediate species. In particular EPR confirms the presence of NO^2? paramagnetic centers and shows two novel N centered paramagnetic centers. A decrease of the degradation rate is observed with increase of carboxylic acid chain length.     

Properties of pulse electrodeposited copper gallium sulphide films

Copper gallium sulphide films were deposited for the first time by the pulse electrodeposition technique at different duty cycles in the range of 6–50 % at room temperature and at a constant current density of 1.0 mA cm^?2. The films exhibited single phase copper gallium sulphide. The grain size increased from 30 to 70 nm with increase of duty cycle. Optical band gap of the films varied in the range of 2.30–2.36 eV. The resistivity increased from 0.10 to 1.70 ohm cm with increase of duty cycle from 6 to 50 %. Preliminary studies on solar cells with p-CuGaS₂/n-CuInS₂ junction yielded an efficiency of 4.14 %. This is the first report on solar cells using CuGaS₂ with CuInS₂.     

Synthesis and optical characterization of copper nanoparticles prepared by laser ablation

The remarkable size-tunable properties of nanoparticles (NPs) make them a hot research topic with applications in a wide range of fields. Hence, copper (Cu) colloidal NPs were prepared using laser ablation (Nd:YAG, 1064 nm, 7 ns, 10 Hz, 6000 pulses) of a copper metal plate at different laser fluences (LFs) in the range of 1–2.5 J cm^?2 in ethylene glycol (EG), at room temperature. Analysis of NPs was carried using different independent techniques such as ultraviolet–visible (UV–vis) spectroscopy; transmission electron microscopy (TEM) and Fourier transform infrared (FTIR) spectroscopy. TEM analysis showed that the NPs were spherical with a bimodal distribution and an average particle size of 5 and 16 nm influence of 1.2 J cms^?2, and 9 and 22 nm at 2 J cm^?2. The UV–vis spectra of colloidal NPs revealed the maximum absorbance at around 584 nm, indicating the formation of Cu NPs, which supported using FTIR spectra. Furthermore, the absorption spectra confirmed the metallic nature of Cu NPs. FTIR spectroscopy was utilized to verify information about the NPs surface state and chemical bonds constructed in the atom groups apparent on their surface.