Abstract:In this work, a set of nanoparticles of Nb 2 O 5 nanoparticles were grown by both the Pechini and the sol-gel methods. The amorphous materials were calcined at 650 • C or at 750 • C. X-ray diffraction, scanning electron microscopy, luminescence and Raman spectroscopy were used in order to characterize the materials. From the study, it is possible to state that the method of production of nanoparticles, beyond the temperature of synthesis, has a great influence on whether the phase produced is hexagonal or orthorhombic. Additionally, compared to de Sol-gel method, the Pechini method produced samples with smaller particle sizes. The photoluminescence spectra of niobium pentoxide nanostructure materials show that the emission peaks are positioned between 334 to 809 nm and there is a change of intensity which varies depending on the synthesis route used. High pressure Raman spectra at room temperature were obtained from two samples grown by the sol-gel method. Up to 6 GPa, where it is possible to observe the Raman bands, no modification other than the increase of disorder was observed, and this can be associated with a change of phase.
Copper oxide (CuO) has been broadly used in different technological and biological applications. However, based on the literature review, there are few reports describing the synthesis of tungsten doped copper oxide and its biological applications, although CuO and W (tungsten) based nanomaterials have been reportedly already synthesized. In this study we synthesized novel CuO and CuO/W (at.1%, 2% and 4%) nanoparticles and explored their tungsten content-dependent bactericide activity. In order to obtain the materials, was used a co-precipitation method which is of low cost. The synthesized materials were characterized by x-ray diffraction (XRD); XRD results indicated that only the sample with at.1% of W presented pure Tenorite phase. Diffuse reflectance spectroscopy (DRS) allowed to obtain the band gap energy values; CuO/W (at.2%) sample exhibited the minimum value of 2.62 eV. Grains sizes ranging from 39.78 to 53.47 nm were established through field emissionscanning electronic microscopy (FE-SEM), and these sizes were confirmed by transmission electron microscopy (TEM). Doping with W also influenced the morphology obtained in all cases. BET (Brunauer, Emmett, Teller) analysis allowed to establish an increase in specific surface area and pore size with W doping. The particle size was determined by dynamic light scattering (DLS). The bactericidal properties were tested using well diffusion method for Escherichia coli and Staphylococcus aureus bacteria. Bactericide response of CuO nanoparticles was improved by the inclusion of W dopant into the CuO structure, leading to an expansion in the inhibition zone for the CuO/W (at.1%) sample; inhibition halo diameters were 1.5 and 12 mm for CuO and CuO/W (at.1%), respectively. Hence, it was possible to
The synthesis of undoped cobalt oxide and cobalt oxide with 4%nickel doping is studied in samples obtained through hydrothermal technique. After the final heat treatment at 300°C, X-ray diffraction analysis indicated the formation of cobalt spinel oxide with a complete replacement of nickel in the lattice. An average crystallite size of ~42 nm and ~31nm was found, as well as a particle size of ~ 20 nm and ~30 nm for Co3O4 and Co3-xNixO4, respectively. Structural parameters were established through Rietveld refinement with a good correspondence between the simulated and the experimental pattern with values of x2 = 1.25 and GOF = 0.90 for Co3O4. The energy band gap was found through UV-Vis spectroscopy in two different regions: Eg1 and Eg2 values vary between 1.54 and 2.04eV for samples doped with nickel. The SEM results indicated the formation of nanostructures with semi-cubic shape and irregular rods. Parameters such as crystal size, particle size, surface area, as well as morphology of the final product depend on doping.
In order to improve the photocatalytic effect of Nb2O5, manganese from 1% to 10% was added by the polymeric precursor’s method. The samples obtained were subjected to different calcination temperatures from 400 to 700 °C. Characterization of the synthesized materials was performed by XRD, IR, Raman and Diffuse Reflectance Spectroscopy (DRS) spectroscopy, FE-SEM, Brunauer–Emmett–Teller (BET) method, Photoluminescence (PL) and Dynamic Light Scattering (DLS). Photocatalytic performance for degradation of Rhodamine B was also evaluated. The Rietveld refined X-Ray Diffraction (XRD) pattern of Nb2O5:Mn 1.0 wt.% (700 °C) sample was similar to that of the un-doped oxide, therefore indicating that Nb was replaced by Mn and, consequently, there are not significant variations in the oxide structure. The Nb2O5:Mn 10.0 wt.% (700 °C) sample has the lowest band gap energy. The specific surface area (SBET) PL value increased as manganese concentration increased. The Nb2O5:Mn 5.0 wt.% (700 °C) sample has an Eg of 3.15 eV and morphological and surface characteristics that made it an appropriate photocatalyst in the Rhodamine B degradation. The novelty of this work relies on the use of a small quantity of Mn ions as dopants leading to Nb2O5:Mn nanostructured particles without using any surfactant or other additives.
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