Highly stable poly(N-vinyl-2-pyrrolidone) (PVP) protected copper nanoparticles were prepared using a simple
chemical reduction route in different solvents {N,
N-dimethyl formamide (DMF) and formamide (FA)} under
aerated condition. The particles were characterized using TEM, SEM, XRD, and UV−visible spectroscopic
techniques. Copper nanostructures of varying shapes and sizes were obtained using hydrazine hydrate as the
reducing agent in both DMF and FA. However, reducing by ascorbic acid in FA leads to formation of mostly
spherical copper nanoparticles with a narrow size distribution. The Cu nanoparticles serve as effective catalyst
for 1,3-dipolar cycloaddition reactions between terminal alkynes and azides to synthesize 1,2,3-triazoles in
excellent yields under mild reaction conditions. The nanocatalysts can be recycled and reused several times
without significant loss of their catalytic activity.
FTIR, Raman, and surface-enhanced Raman scattering (SERS) of methimazole (MMI) have been investigated. MMI is an important antithyroid drug that inhibits the formation of thyroid hormone. It is widely used clinically in the treatment of hyperthyroidism, and thus it is useful to study its surface adsorption characteristics. The experimental FTIR and Raman data are supported with DFT calculations using B3LYP functional with LANL2DZ basis set. This is the first report on the vibrational analysis of the thiol and thione forms of MMI and their various possible silver complexes. pH-dependent normal Raman spectra have been recorded, which show the abundance of the thione form of MMI in acidic, neutral, and alkaline media. From the SERS spectra as well as theoretical calculations, it has been inferred that in neutral and alkaline media, the thiol form of MMI is chemisorbed to the silver surface through the ring N atom of the imidazole ring with an edge-on orientation and the imidazole ring lying in the plane of the silver surface. In contrast, it has been concluded that in the acidic medium, the thione form of MMI gets adsorbed to the silver surface. Thus, the pH-dependent SERS spectra have shown the preferential existence of thione and thiol tautomeric forms on the silver surface in acidic, neutral, and alkaline media.
The reduction of silver ions in formamide is shown to take place spontaneously at room temperature without addition of any reductant. The growth of Ag particles was found to be dependent on Ag+ ion concentration. In the absence of any stabilizer, deposition of silver film on the glass walls of the container takes place. However, in the presence of poly(N-vinyl-2-pyrrolidone) (PVP) or colloidal silica (SiO2), which are capable of stabilizing silver nanoparticles by complexing and providing support, a clear dispersion was obtained. The formation of the silver nanoparticles under different conditions was investigated through UV-visible absorption spectrophotometry, gas chromatography, and also electron and atomic force microscopic techniques. Atomic force microscopy results for silver films prepared in the absence of any stabilizer showed the formation of polygonal particles with sizes around 100 nm. Transmission electron microscopy results showed that the prepared silver particles in the presence of PVP were around 20 nm. The Ag nanoparticles get oxidized in the presence of chloroform and toluene. Surface modification of silver film was done in the presence of the tetrasodium salt of ethylenediaminetetraaceticacid (Na4EDTA). It was shown that the reactivity of the silver film increased in its presence. The Fermi potential of silver particles in the presence of Na4EDTA seems to lie between -0.33 and -0.446 V vs NHE.
Room temperature synthesis of silver nanoparticles has been successfully achieved by adding NaOH acting as an accelerator for the reduction of silver ions in ethylene glycol and glycerol without adding any external reducing agent. Highly monodisperse silver particles are obtained in the presence of various stabilisers such as PVP, SiO 2 and SDS. Nanoparticles with a mean diameter of 25 nm and a mean deviation of 2 nm could be obtained under experimental conditions. The silver nanoparticles so obtained could be easily transferred to chloroform containing CTAB, giving rise to CTAB stabilised silver nanoparticles having sizes of around 25 nm. The newly found role of OH -stabilisation was used to formulate a mechanism for the formation of silver nanoparticles in ethylene glycol and glycerol. In this mechanism, silver nanoparticles are stabilised in ethylene glycol by the adsorbed OH -ions.
A facile route for in situ synthesis of Co and Ni nanoparticles in a preorganized polyacrylamide gel is reported. Metal-polymer composites were prepared by gamma-irradiation at room temperature. The Co nanoparticles were roughly 3-5 nm in size and were stable in the polymer matrix in the presence of air. The presence of Co and Ni nanoparticles was established by their ability to transfer an electron to methyl viologen {paraquat: 1,1'-dimethyl 4,4'-dipyridinium dichloride; MV(2+) (Cl(-))(2)}. The Co and Ni nanoparticles were probed for their magnetic characteristics by a superconducting quantum interferometer device (SQUID) magnetometer and display a low superparamagnetic blocking temperature T(B) of about 13 and 10 K, respectively. The field-dependent magnetic behavior below T(B) displays the standard features corresponding to superparamagnetism, as expected for very small Co and Ni crystallites. This also suggests that particles are polycrystalline in nature.
Nanoparticles of titanium dioxide were prepared using the sol-gel method without any impurity. Rietveld refinement of XRD data confirmed the anatase phase of synthesized nanoparticles with space group I4 1/ amd (141). XRD pattern revealed the crystalline nature of synthesized nanopowder. The average crystallite size of synthesized nanoparticles was calculated 7.5 nm. The electrochemical performance of synthesized TiO 2 nanopowder was investigated as working electrode. The electrochemical reaction was found diffusion-controlled as observed from cyclic voltammetry (CV) studies at different scan rates. The diffusion-controlled charge storage mechanism also confirmed by charge transfer resistance and Warburg impedance, as calculated from the EIS analysis. SEM micrograph showed the plate-like structure grown in cluster cloud of particles of synthesized TiO 2 nanocrystals. Absorbance and optical bandgap were obtained using UV-Vis spectra. De-convoluted PL spectra provided the emission pattern from the ultra-violet region to green region due to the presence of interstitial oxygen vacancies. The tune bandgap with EIS measurements of synthesized TiO 2 nanoparticles offers its potential application in energy storage devices and photovoltaic applications.
K E Y W O R D SAnatase TiO 2 , CV studies, EIS, PL emission, X-ray diffraction
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