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In this contribution we report on the synthesis of n-type Bismuth vanadate (BiVO4) nanorods prepared via the use of aqueous extracts of Callistemon viminalis. X-ray diffraction analysis confirmed the formation of highly crystalline monoclinic BiVO4 nanorods post annealing of the Bismuth vanadate precursor powder at 500 °C. Scanning Electron Microscopy and High Resolution Transmission Electron Microscopy showed that BiVO4 nanorods have a high aspect ratio. Using UV-Vis absorption measurements the optical band gap of the nanorods is estimated to be 2.4 eV which makes the bio-synthesized BiVO4 powder a good candidate for sunlight driven photocatalysis.
This work reports on the synthesis and the main physical and chemical properties of ZnO nanoparticles synthesized by an entirely green Bio-physical-chemical process using natural dye extract from Adansonia digitata leaves as an efficient reduction/oxidizing agent. Their structural and surfaces properties by electron microscopy, X-rays diffraction, Raman and TGA, as well as gas adsorption analysis are reported.
Vanadium dioxide thin films are considered as smart functional coatings for thermal shielding, and are attractive as a passive thermal shield for spacecrafts. In space they would, however, be subjected to bombardment by interstellar dust particles and electromagnetic radiation. Materials subjected to irradiation will suffer damages induced by the displacement cascades initiated by nuclear reaction. Such cosmic radiation can severely impact the structure and function of materials. To study this effect in the laboratory, we have deposited VO2 films on silicon wafers and exposed them to γ-radiation of doses up to 100 kGy by using a 60Co nuklid source with 1.17 and 1.33 MeV photon energy. We anticipate that the γ-radiation causes local structural perturbations which can amount to defects with a corresponding change in electronic structure and thermal shielding property. We report on the photo emission spectroscopy of gamma irradiated VO2 thin films.
Chitosan is a polymeric compound with functional groups which enable surface binding to nanoparticles and antibacterial activity. The antimicrobial activity was studied using silver nanoparticles with varied concentrations of chitosan. The nanoparticles were synthesized through a simple and environmentally friendly method at room temperature. Spherical particles with average sizes between 2 and 6 nm were obtained and their crystallinity showed a face-centered cubic phase. The evidence of chitosan presence on the nanoparticle surface was confirmed by the characteristic diffraction peak of chitosan and by FTIR spectra where the bonding of amine group could be depicted. The chitosan-capped silver nanoparticles showed good antibacterial and antifungal activities with MIC values between 0.20 and 1.5 mg.mL-1 compared to those obtained from most of references (up to 6.25 mg.mL-1) on the selected gram-positive (Staphylococcus aureus, Enterococcus faecalis), gram-negative (Klebsiella pneumoniae, Pseudomonas aeruginosa ) bacteria and fungi (Candida albicans, Cryptococcus neoformans).
Synthesis and characterization of cassava bark nanoparticles (CBNPs) was carried out using ball milling at 36, 48, 60 and 72 hours. The morphology study was done using SEM and the Gwyddion software was used to determine the particle sizes from the SEM images. The particle distribution for the un-milled cassava bark (CB) was between 1.25 + 0.06 to 19.92 + 1.00 µm, while after milling for 36, 48, 60 and 72 hours the average particle size were 4.07 + 0.20, 4.00 + 0.20 µm, 80.90 + 4.05, 74.50 + 3.73 nm respectively. 13.68 + 0.68 nm was obtained by XRD using Scherrer equation after milling for 72 hours and the XRD results revealed the presence of compounds such as SiO2, CaCO3 and KAlSi3O8. TEM was used to determine nanoparticle size distribution after milling for 72 hours and the particle size ranged from 9.73 + 0.49 to 114.60 + 5.73 nm for cassava bark nanoparticles (CBNPs), EDX results showed trace element of Si, Ca, K, Fe, Al, O in the CB milled for 72hours.
This article aims to prepare high quality of TiO2 powder and study the effect of annealing temperature. TiO2 particles were synthesized by sol-gel method using titanium tetra chloride (TiCl4) as a precursor. The dried gel was annealed at temperatures of 500oC, 600oC, 700°C and 800 °C each for 4 hours. The as-prepared samples were further characterized using X-Ray diffraction (XRD), Scanning electron microscope (SEM), Energy dispersive X-ray Fluorescence spectrometer (EDX), XRD showed anatase structure after annealing and its diffraction scattering intensity indicated the improvement in the crystal structure quality of TiO2 as the temperature increases. SEM micrographs showed a randomly distributed and non-uniform cluster of TiO2 that has a size increase with annealing temperatures. EDX indicated stoichiometric chemical composition between Ti and O enhanced by annealing.
The synthesis of Platinum (Pt) nanoparticles by gamma irradiation is presented. The 0.1 M Pt solution of different concentration was prepared from K2PtCl4. The platinum aqueous solutions were irradiated by gamma radiation at a dose of 70, 90 and 120 kGy. The findings show the effect of irradiation on PtII solutions with different concentrations. The big black particles that are fairly agglomerated when the concentration was above 0.0050 M were observed. The UV-Vis spectrum of Pt of different concentrations shows a strong absorption peak at the wavelength 261 nm after irradiation, which indicates the presence of platinum nanoparticles. Furthermore, FTIR, XRD and HRTEM images also confirmed the presence of the nanoparticles produced by Radiolysis. The size of the Pt nanoparticles was found to be 7.39 nm.
A novel synthesis of Al (1xxx)/carbonised coconut shell (CCS) nanoparticles using a ball milling technique was investigated. Initial Al/0.1%CCS powders of an average size of 51.06μm was milled for a period of 70 h. The milled particles at 16, 46 and 70 h were characterized using X-ray diffractomer (XRD), scanning electron microscope (SEM), transmission electron microscope and UV-Vis spectrophotometer. Result revealed that the calculated particle crystallite size from XRD aided with Scherrer’s equation is consistent with particle image sizes obtained from SEM aided with software. TEM image depicted variation in orientation and appearance of the Al 1xxx/0.1% CCS nanoparticles at different milling time. The wide variation in the particle size is attributable to different ball impacts on the individual powders during the ball milling process. Increased maximum absorbance observed with the milled particles when compared with the initial powders is an indication of quantum/nanosizing effect due to ball milling.
Graphene nanosheets were prepared by pulsed Nd:YAG laser ablation of graphite target in H2O under ambient conditions. The synthesized graphene nanosheets were characterized by high resolution transmission electron microscope (HRTEM), X-ray diffraction (XRD), Raman spectroscopy and Selected Area Electron Diffraction (SAED). The obtained structural and morphological analysis confirmed that the graphene nanosheets could be formed in an aqueous medium via one step method where a nanosecond pulsed near-infrared (NIR) laser (λ = 1064 nm) is used to ablate the surface of a pure graphite target. Compared to other used chemical methods to synthesis graphene nanosheets, laser ablation is an easy, versatile, environmental friendly and rapidly growing method for the synthesis of nanostructured materials such as graphene nanosheets. This technique showed normal operation in liquid medium (i.e. water or organic) under ambient conditions. Our study confirmed the great potential of laser ablation in liquid method for the fabrication of graphene nanosheets based nanofluids wich has a potential applicatiuon as a heat transfer fluid.
Nanosized CeO2-CuO (CeCu, 2:1) and CeO2-CoO (CeCo, 2:1) were synthesized by co-precipitation from nitrate precursors using 25% ammonia solution (NH4OH) as the precipitating agent. The catalysts were calcined in air at 800°C for 4h to evaluate the thermal stability. Powder x-ray diffraction (XRD) and Dynamic Light Scattering (DLS) techniques were used for catalyst characterization. A Thermo Gravimetric/Differential Thermal Analyzer (TG/DTA) was used to determine the catalytic efficiency and soot oxidation activity. Ce-composite nanoparticles heightens the redox properties of the catalyst relative to undoped ceria. The Ce-composite samples exhibited excellent soot catalytic combustion performance by decreasing activation energy of soot oxidation.
The effects of different starting materials using nano-synthesis methodology on electrochemical performance of lithium manganese oxide (LixMn2O4) are studied. Four spinel-type LixMn2O4 (LMO) cathode materials were prepared with different lithium and manganese sources and were analyzed chemically and characterized by BET and XRD. The electrochemical performance of the cathodes at room temperature and elevated temperature was tested. The crystal structure was indexed to be a cubic system with lattice parameters of 8.2342 ±0.170 Å and defined to the space group Fd3m. There was no peak of impurity because the raw materials for Mn source were first treated with acid. Although the results showed that the structures of the samples were confirmed to be cubic spinel structure, the lattice parameter and specific surface area of the samples were different. The LiMn2O4 cathodes have an initial discharge capacity of over 120mAh/g and show an ordinary two-step voltage profile. The results demonstrated that the cathode materials prepared with LiNO3 as Li source have larger lattice parameters, than those prepared from LiOH·H2O as Li source. The cathode prepared from Electrochemical Manganese Dioxide (EMD) as Mn source have larger particle sizes, lower first charge and discharge capacity, better cyclic performance, whereas those from Chemical Manganese Dioxide (CMD) as Mn source have smaller particle size, higher first charge and discharge capacity, and poor cyclic stability at elevated temperature. The cell polarization of the cathode developed by LiOH•H2O and EMD was identified to be the least and the elevated temperature cycelability to be the best. These manifestations can be attributed to differences in Li and Mn sources, specific surface areas, purities of starting materials and synthesis conditions. Melt-impregnation as a nano-synthesis method proved to be an excellent method to synthesize LiMn2O4 cathode materials that can operate at elevated temperatures when using correct starting materials and good control of synthesis temperatures.
Research focus in recent years on magnetic behaviour of transition metal (TM) ions embedded in semiconductors has shifted from intrinsic effects to extrinsic effects such as the formation of nanoclusters of the TM ions and the influence of the host matrix on their magnetic behaviour. Our studies, using conversion electron Mössbauer Spectroscopy and magnetization measurements, on SiO2 and Al2O3 substrates implanted with 4 at. % Fe, show ferromagnetic behaviour of α-Fe clusters in amorphous SiO2, but α-Fe2O3 clusters displaying superparamagnetic relaxation in crystalline Al2O3.
This contribution reports, to the best of our knowledge, for the first time on the neutron tunneling phenomenon in nickel isotopes based nanostructured. More accurately, 58Ni-62Ni-58Ni thin films Fabry-Perot resonator configuration exhibited several tunneling resonances. In total, there were 7 tunneling resonances. These tunneling resonances manifest themselves via sharp dips in the total reflection plateau due to quasi-bound states in the nanostructured isotopic based nickel thin film Fabry-Perot resonator.
In this study we investigate the motion of a torsionally restrained beam used in tapping mode atomic force microscopy (TM-AFM), with the aim of manufacturing at nano-scale. TM-AFM oscillates at high frequency in order to remove material or shape nano structures. Euler-Bernoulli theory and Eringen’s theory of non-local continuum are used to model the nano machining structure composed of two single degree of freedom systems. Eringen’s theory is effective at nano-scale and takes into account small-scale effects. This theory has been shown to yield reliable results when compared to modelling using molecular dynamics.
The system is modelled as a beam with a torsional boundary condition at one end; and at the free end is a transverse linear spring attached to the tip. The other end of the spring is attached to a mass, resulting in a single degree of freedom spring-mass system. The motion of the tip of the beam and tip mass can be investigated to observe the tip frequency response, displacement and contact force. The beam and spring–mass frequencies contain information about the maximum displacement amplitude and therefore the sample penetration depth and this allows
We report on the formation of gamma phase cuprous iodide (CuI) thin films of various film thickness with high (111) orientation deposited by vacuum thermal evaporation of powders attained through a cost-saving extraction method. The study investigated the dependence of structural and optoelectronic properties of the thin films on film thickness. Structural characterisation of the films revealed an increase in crystallite size and a decrease in dislocation density with film thickness which indicated an improvement in the crystallographic microstructure. There was a strong orientation towards (111) growth. The Scanning Electron Microscope images of the CuI thin films showed a compact morphology with an increase in larger grains as film thickness increased. The thin films showed a mean optical transmittance of around 70 % in the visible region with a decreasing trend as thickness increased. There was an observed red shift of the transmittance spectra with film thickness. All thin films also showed good electrical conductivity. However, the figure of merit improved with decreasing thickness. The good optical transmittance and relatively low resistivity qualify the CuI thin films as candidates for electro-optical device applications.
Pure and transition metal (TM)-doped ZnO nanocrystals were synthesized using a wet-chemical process. Synthesis was carried out in distilled water at 85 °C followed by calcining the as-prepared powders at 280 °C and 600 °C. Co, Mn and Fe doping at 4 and 8 mol % was achieved by adding CoCl2.6H2O, MnCl2 .4H2O and FeCl2 .4H2O respectively during the synthesis. Crystal phase characterization was carried out by X-ray powder diffraction (XRD) which confirmed the formation of ZnO in the wurtzite polymorph. The band gap energy of the nanocrystals was measured by both photoluminescence spectroscopy (using the Near Band Edge Emission) and UV-Vis absorption spectroscopy, using a modified version of the Tauc law. Widening of the band gap energy from 3.23 eV to 3.33 eV with increased doping concentration was observed for all the dopants. Ab-initio simulations of doped and undoped ZnO crystals using density functional theory as implemented in the Quantum Espresso package confirmed the increase in the band gap energies with doping concentration.
Herein, we report on the syntheses of ZnO nanoparticles using different precursors Zn(NO3)2•6H2O, Zn(CH3COO)2•2H2O, ZnCl2, and ZnSO4.H2O by a microwave assisted method. The different precursors resulted in different structural, optical and photocatalytic degradation of Rhodamine B dye. The nanoparticles resulted in rod-like and pseudo-spherical morphologies when the ZnO2•6H2O, (Zn(CH3COO)2•2H2O and ZnCl2 precursors were used, with the proportion of the spherical morphology in each photocatalyst varying in the order Zn(NO3)2•6H2O > Zn(CH3COO)2•2H2O > ZnCl2. The ZnSO4.H2O precursor yielded trapezium shaped particles that were agglomerated through oriented attachment. For photocatalytic degradation studies, the fastest degradation was achieved using the SNO3- photocatalyst, which degraded the dye in a period of 120 min, followed by SCH3COO- at 150 min, SCl- at 180 min and SSO42- managing to degrade only 15 % of the dye after 240 min. The difference in the activity was attributed to surface area differences, which followed the order SNO3- > SCH3COO- >SCl- > SSO42-, with the photocatalyst that had the highest surface area showing high degradation rates. The high degradation rate observed for the SNO3- photocatalyst was also attributed to the presence of a large number of spherical particles thereby having a larger proportion of the high energy  and [000-1] faces known to be highly active.
This work aims to develop simple and cost-effective methods in reduction of Cr(VI) from water to less toxic and easy separated Cr(III) using Titanium dioxide (TiO2).
TiO2 nanoparticles are prepared by a sol-gel method using titanium tetra-chloride and characterized using X-Ray Diffraction (XRD), Scanning electron microscope (SEM), Energy dispersive X-ray Fluorescence spectrometer (EDX) and UV-visible spectroscopy. XRD shows Anatase structure of TiO2 after annealing at 600°C for four hours. The particles size is estimated to be 70 nm using SEM.UV-Visible spectroscopy indicated that TiO2 nanoparticles played important role in decreasing the concentration of Cr (VI) in water samples for different pH range of 1 to 4. The decrease in Cr(VI) concentration after the treatment is ascribed to the reduction caused by the photocatalyst effect that resulted from the presence of TiO2 nanoparticle in water samples under direct exposure to direct sunlight.
This study investigates the adsorption efficiency of goethite nanostructured powder for the simultaneous removal of cobalt and nickel ions. The nanostructured powder sample was synthesized via a chemical precipitation technique and characterized using SEM, FTIR-ATR and XRD techniques. From batch adsorption studies, maximum absorption for Co(II) and Ni(II) ions occurred at an equilibrium contact time of 80 min, with an adsorbent mass of 0.1 g, and at pH=7. Co(II) ions showed greater affinity to the nanoparticles as compared to Ni(II). The maximum quantities adsorbed were recorded as 148.5 mg/g for Co(II) and 110.6 mg/g for Ni(II) ions. The best isotherm model fit for both metal ions was the Freundlich model indicating heterogeneity of the surface binding sites. The pseudo-second order kinetic model was the best-fit model: an indication of a strong chemical adsorption between the adsorbent surface and metal ions. The findings show that the goethite nanostructured powder is a very effective adsorbent material and prominent candidate for the simultaneous removal of cobalt and nickel ions from water.
The adult Papilio demoleus Linnaeus comes in different sizes (80-100 mm) and colours. On the basis of structural colour observation, an experimental and theoretical study on the different colours on Papilio demoleus Linnaeus wings was conducted. The wing scales were investigated from a photonic crystal perspective using scanning electron and optical microscopies and reflectance measurements. In the SEM measurements, the parts studied show nanostructured ridges separated by crossribs (grooves). The scales show several tilted cuticle layers lapped on the ridges, which constitute a grating. The widths of the ridges and crossribs (grooves) in the grating are different. Arrangements and shapes of scales are clearly seen under the optical microscopy. It was deduced that the yellow colour with the highest reflectance of 485 nm and 580 nm could be due to multiple interferences from a highly tilted cuticle arrangement. The layer arrangement in the brown and ash scales is not enough to reflect observable interference light. The study shows an application in fine light elements in the photo-electro devices.