Indium tin oxide (ITO) and titanium dioxide (TiO2) anti-reflective coatings (ARCs) were deposited on a (100) P-type monocrystalline Si substrate by a radio-frequency (RF) magnetron sputtering. Polycrystalline ITO and anatase TiO2 films were obtained at room temperature (RT). The thickness of ITO (60 to 64 nm) and TiO2 (55 to 60 nm) films was optimized, considering the optical response in the 400- to 1,000-nm wavelength range. The deposited films were characterized by X-ray diffraction (XRD), Raman spectroscopy, field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS), and atomic force microscopy (AFM). The XRD analysis showed preferential orientation along (211) and (222) for ITO and (200) and (211) for TiO2 films. The XRD analysis showed that crystalline ITO/TiO2 films could be formed at RT. The crystallite strain measurements showed compressive strain for ITO and TiO2 films. The measured average optical reflectance was about 12% and 10% for the ITO and TiO2 ARCs, respectively.
Ag/PMMA nanocomposites were successfully synthesized by in-situ technique. Transmission electron microscopy (TEM) images show that the particles are spherical in shape and their sizes are dependent on temperature. The smallest particle achieved high stability as indicated from Zeta sizer analysis. The red shift of surface plasmon resonance (SPR) indicated the increases of particle sizes. X-ray diffraction (XRD) patterns exhibit a two-phase (crystalline and amorphous) structure of Ag/PMMA nanocomposites. The complexation of Ag/PMMA nanocomposites was confirmed using Raman spectroscopy. Fourier transform infrared spectroscopy spectra confirmed that the bonding was dominantly influenced by the PMMA and DMF solution. Finally, thermogravimetric analysis (TGA) results indicate that the total weight loss increases as the temperature increases.
This article reviews progress in the application of electrophoretic techniques for the separation of nanoparticles. Numerous types of nanoparticles have recently been synthesised and integrated into different products and procedures. Consequently, analytical methods for the efficient characterisation of nanoparticles are now required. Several studies have revealed that gel electrophoresis can readily be used for separating nanoparticles according to their size or shape. However, many other studies focused on separation of nanoparticles by CE. In some cases nanoparticles could be separated by CZE, simply using pure buffer as the BGE. In other studies, buffer additives (most often SDS) were used, enabling fast separations of metallic nanoparticles by size. Other CE methods also allowed for separation of nanoparticle conjugates with biomolecules. Dielectrophoresis is yet another electrophoretic technique useful in separation and characterisation of nanoparticles; particularly nanotubes. Detection methods often used after electrophoretic separation include UV/Vis absorption and fluorescence spectroscopy. Examples of recent and relevant older reports are presented here. The authors conclude that electrophoretic methods for nanoanalysis can provide inexpensive and efficient tools for quality assurance and safety control; and as a consequence, they can augment transfer of nanotechnologies from research to industry.
Graphene (Gr)/gold (Au) and graphene-oxide (GO)/Au nanocomposites (NCPs) were synthesized by performing pulsed-laser-induced photolysis (PLIP) on hydrogen peroxide and chloroauric acid (HAuCl4) that coexisted with Gr or GO in an aqueous solution. A 3-month-long aqueous solution stability was observed in the NCPs synthesized without using surfactants and additional processing. The synthesized NCPs were characterized using absorption spectroscopy, transmission electron microscopy, Raman spectroscopy, energy dispersive spectroscopy, and X-ray diffraction to prove the existence of hybrid Gr/Au or GO/Au NCPs. The synthesized NCPs were further evaluated using the photocatalytic reaction of methylene blue (MB), a synthetic dye, under UV radiation, visible light (central wavelength of 470 nm), and full spectrum of solar light. Both Gr/Au and GO/Au NCPs exhibited photocatalytic degradation of MB under solar light illumination with removal efficiencies of 92.1% and 94.5%, respectively.
A gold nanoparticle (AuNP) has a localized surface plasmon resonance peak depending on its size, which is often utilized for surface-enhanced Raman scattering (SERS). To obtain information on the cholesterol (Chol)-incorporated lipid membranes by SERS, AuNPs (5, 100 nm) were first functionalized by 1-octanethiol and then modified by lipids (AuNP@lipid). In membrane surface-enhanced Raman spectroscopy (MSERS), both signals from 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC) and Chol molecules were enhanced, depending on preparation conditions (size of AuNPs and lipid/AuNP ratio). The enhancement factors (EFs) were calculated to estimate the efficiency of AuNPs on Raman enhancement. The size of AuNP100nm@lipid was 152.0 ± 12.8 nm, which showed an surface enhancement Raman spectrum with an EF2850 value of 111 ± 9. The size of AuNP5nm@lipid prepared with a lipid/AuNP ratio of 1.38 × 104 (lipid molecule/particle) was 275.3 ± 20.2 nm, which showed the highest enhancement with an EF2850 value of 131 ± 21. On the basis of fluorescent probe analyses, the membrane fluidity and polarity of AuNP@lipid were almost similar to DOPC/Chol liposome, indicating an intact membrane of DOPC/Chol after modification with AuNPs. Finally, the membrane properties of AuNP@lipid systems were also discussed on the basis of the obtained MSERS signals.
Carbon nanotube-quicklime nanocomposites (CQNs) have been synthesized via the chemical vapor deposition (CVD) of n-hexane using a nickel metal catalyst supported on calcined carbonate stones at temperatures of 600-900 °C. The use of a Ni/CaO(10 wt%) catalyst required temperatures of at least 700 °C to obtain XRD peaks attributable to carbon nanotubes (CNTs). The CQNs prepared using a Ni/CaO catalyst of various Ni contents showed varying diameters and the remaining catalyst metal particles could still be observed in the samples. Thermogravimetric analysis of the CQNs showed that there were two major weight losses due to the amorphous carbon decomposition (300-400 °C) and oxidation of CNTs (400-600 °C). Raman spectroscopy results showed that the CQNs with the highest graphitization were synthesized using Ni/CaO (10 wt%) at 800 °C with an IG/ID ratio of 1.30. The cyclic voltammetry (CV) of screen-printed carbon electrodes (SPCEs) modified with the CQNs showed that the performance of nanocomposite-modified SPCEs were better than bare SPCEs. When compared to carboxylated multi-walled carbon nanotubes or MWNT-COOH-modified SPCEs, the CQNs synthesized using Ni/CaO (10 wt%) at 800 °C gave higher CV peak currents and comparable electron transfer, making it a good alternative for screen-printed electrode modification.
In this study, the impact of different oxidizing agents on the structural integrity of activated carbon (AC) and multiwalled carbon nanotubes (MWCNTs) was studied for the removal of BTX from aqueous solution. Seven different combinations of green oxidizing agents (mild organic acids) in conjugation with NaOCl (basic oxidizing agent) were used. The modified adsorbents were analyzed by Brunauer, Emmett, and Teller (BET) surface area analyzer, Fourier transform infrared spectroscopy (FTIR), Boehm titration, Raman spectroscopy, thermal gravimetric analysis (TGA), x-ray diffraction (XRD), zeta potential, and variable pressure field emission scanning electron microscope (VPFESEM). The results suggested that the carbonaceous sorbents modified with combination of citric acid tartaric acid, malic acid and salicylic acid (CTMS-I) showed increased surface area (O-AC: 871.67 m2/g, O-MWCNTs: 336.37 m2/g) and total pore volume (O-AC: 0.59 cm3/g, O-MWCNTs: 0.04 cm3/g), with the significantly improved thermal stability. Preliminary batch adsorption experiments conducted using the present prepared O-AC and O-MWCNTs, showed an improved performance towards the adsorption of BTX, compared with other available reported adsorbents in the literature.
Gamma-ray radiation was used as a clean and easy method for turning the physicochemical properties of graphene oxide (GO) in this study. Silane functionalized-GO were synthesized by chemically grafting 3-aminopropyltriethoxysilane (APTES) and 3-glycidyloxypropyltrimethoxysilane (GPTES) onto GO surface using gamma-ray irradiation. This established non-contact process is used to create a reductive medium which is deemed simpler, purer and less harmful compared conventional chemical reduction. The resulting functionalized-GO were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TGA), and Raman spectroscopy. The chemical interaction of silane with the GO surface was confirmed by FT-IR. X-ray diffraction reveals the change in the crystalline phases was due to surface functionalization. Surface defects of the GO due to the introduction of silane mioties was revealed by Raman spectroscopy. Thermogravimetric analysis of the functionalized-GO exhibits a multiple peaks in the temperature range of 200-650 °C which corresponds to the degradation of chemically grafted silane on the GO surface.
A tin oxide (SnO2) and reduced graphene oxide (rGO) hybrid composite gas sensor for high-performance carbon dioxide (CO2) gas detection at room temperature was studied. Since it can be used independently from a heater, it emerges as a promising candidate for reducing the complexity of device circuitry, packaging size, and fabrication cost; furthermore, it favors integration into portable devices with a low energy density battery. In this study, SnO2-rGO was prepared via an in-situ chemical reduction route. Dedicated material characterization techniques including field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray (EDX) spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) were conducted. The gas sensor based on the synthesized hybrid composite was successfully tested over a wide range of carbon dioxide concentrations where it exhibited excellent response magnitudes, good linearity, and low detection limit. The synergistic effect can explain the obtained hybrid gas sensor's prominent sensing properties between SnO2 and rGO that provide excellent charge transport capability and an abundance of sensing sites.
A rapid, sustainable, and ecologically sound approach is urgently needed for the production of semiconductor nanomaterials. CuSe nanoparticles (NPs) were synthesized via a microwave-assisted technique using CuCl2·2H2O and Na2SeO3 as the starting materials. The role of the irradiation time was considered as the primary concern to regulate the size and possibly the shape of the synthesized nanoparticles. A range of characterization techniques was used to elucidate the structural and optical properties of the fabricated nanoparticles, which included X-ray diffraction, energy-dispersive X-ray spectroscopy (EDX), atomic force microscopy, field emission scanning electron microscopy, Raman spectroscopy (Raman), UV-Visible diffuse reflectance spectroscopy (DRS), and photoluminescence spectroscopy (PL). The mean crystallite size of the CuSe hexagonal (Klockmannite) crystal structure increased from 21.35 to 99.85 nm with the increase in irradiation time. At the same time, the microstrain and dislocation density decreased from 7.90 × 10-4 to 1.560 × 10-4 and 4.68 × 10-2 to 1.00 × 10-2 nm-2, respectively. Three Raman vibrational bands attributed to CuSe NPs have been identified in the Raman spectrum. Irradiation time was also seen to play a critical role in the NP optical band gap during the synthesis. The decrease in the optical band gap from 1.85 to 1.60 eV is attributed to the increase in the crystallite size when the irradiation time was increased. At 400 nm excitation wavelength, a strong orange emission centered at 610 nm was observed from the PL measurement. The PL intensity is found to increase with an increase in irradiation time, which is attributed to the improvement in crystallinity at higher irradiation time. Therefore, the results obtained in this study could be of great benefit in the field of photonics, solar cells, and optoelectronic applications.
Graphene oxide/Cuprous oxide (GO/Cu₂O) composite is a visible light photocatalyst for the degradation of dyes. A simple and efficient approach for preparing GO/Cu₂O composite adopted in this study involves reducing cuprous oxide precursors in the presence of graphene oxide using an aqueous solution of pulp derived from banana fruit. The GO/Cu₂O composite was characterized by Fourier transform infrared spectroscopy (FT-IR), Diffused reflectance Ultraviolet visible spectroscopy (DRS UV-Vis), Raman spectroscopy and Field Emission Scanning electron microscopy (FE-SEM). Cu₂O particles were distributed randomly on the graphene oxide sheets due to the template effect of GO. The results showed higher photocatalytic activity for the composite (band gap 2.13 eV), for the degradation of the organic dyes (Methylene blue and Rhodamine-B). The enhanced photocatalytic activity is due to effective charge transfer from GO to Cu₂O, and high specific surface area which improves the effective separation of the generated electron-hole pairs. Our present study is inspired by a facile, low cost, green production of (GO/Cu₂O) composite whose photocatalytic activity can be extended to degradation of all other water-born textile dyes.
In seabed logging the magnitude of electromagnetic (EM) waves for the detection of a hydrocarbon reservoir in the marine environment is very important. Having a strong EM source for exploration target 4000 m below the sea floor is a very challenging task. A new carbon nanotubes (CNT) fibres/aluminium based EM transmitter is developed and NiZn ferrite as magnetic feeders was used in a scaled tank to evaluate the presence of oil. Resistive scaled tank experiments with a scale factor of 2000 were carried out. X-ray Diffraction (XRD), Raman Spectroscopy and Field Emission Scanning Electron Microscope (FESEM) were done to characterize the synthesized magnetic feeders. Single phase Ni0.76Mg0.04Zn0.2Fe2O4, obtained by the sol-gel method and sintered at 700 degrees C in air, has a [311] major peak. FESEM results show nanoparticles with average diameters of 17-45 nm. Samples which have a high Q-factor (approximately 50) was used as magnetic feeders for the EM transmitter. The magnitude of the EM waves of this new EM transmitter increases up to 400%. A curve fitting method using MATLAB software was done to evaluate the performance of the new EM transmitter. The correlation value with CNT fibres/aluminium-NiZnFe2O4 base transmitter shows a 152.5% increase of the magnetic field strength in the presence of oil. Modelling of the scale tank which replicates the marine environment was done using the Finite Element Method (FEM). In conclusion, FEM was able to delineate the presence of oil with greater magnitude of E-field (16.89%) and the B field (4.20%) due to the new EM transmitter.
The heterocyclic chalcone containing thiophene ring 1-(4-chlorophenyl)-3-(2-thienyl)prop-2-en-1-one, C13H9ClOS was synthesized and investigated using experimental techniques such as nuclear magnetic resonance (1H and 13C NMR), Fourier transform infrared spectroscopy (FTIR) at room temperature, differential scanning calorimeter (DSC) from room temperature to 500K and Raman scattering at the temperature range 10-413K in order to study its structure and vibrational properties as well as stability and possible phase transition. Density functional theory (DFT) calculations were performed to determine the vibrational spectrum viewing to improve the knowledge of the material properties. A reasonable agreement was observed between theoretical and experimental Raman spectrum taken at 10K since anharmonic effects of the molecular motion is reduced at low temperatures, leading to a more comprehensive assignment of the vibrational modes. Increasing the temperature up to 393K, was observed the typical phonon anharmonicity behavior associated to changes in the Raman line intensities, line-widths and red-shift, in special in the external mode region, whereas the internal modes region remains almost unchanged due its strong chemical bonds. Furthermore, C13H9ClOS goes to melting phase transition in the temperature range 393-403K and then sublimates in the temperature range 403-413K. This is denounced by the disappearance of the external modes and the absence of internal modes in the Raman spectra, in accordance with DSC curve. The enthalpy (ΔH) obtained from the integration of the endothermic peak in DSC curve centered at 397K is founded to be 121.5J/g.
The potential combination of two nondestructive techniques, that is, Raman spectroscopy (RS) and attenuated total reflectance-fourier transform infrared (ATR-FTIR) spectroscopy with Pearson's product moment correlation (PPMC) coefficient (r) and principal component analysis (PCA) to determine the actual source of red gel pen ink used to write a simulated threatening note, was examined. Eighteen (18) red gel pens purchased from Japan and Malaysia from November to December 2014 where one of the pens was used to write a simulated threatening note were analyzed using RS and ATR-FTIR spectroscopy, respectively. The spectra of all the red gel pen inks including the ink deposited on the simulated threatening note gathered from the RS and ATR-FTIR analyses were subjected to PPMC coefficient (r) calculation and principal component analysis (PCA). The coefficients r = 0.9985 and r = 0.9912 for pairwise combination of RS and ATR-FTIR spectra respectively and similarities in terms of PC1 and PC2 scores of one of the inks to the ink deposited on the simulated threatening note substantiated the feasibility of combining RS and ATR-FTIR spectroscopy with PPMC coefficient (r) and PCA for successful source determination of red gel pen inks. The development of pigment spectral library had allowed the ink deposited on the threatening note to be identified as XSL Poppy Red (CI Pigment Red 112).
Cancer still presents enormous challenges in the medical world. Currently, the search for
anticancer compounds has garnered a lot of interest, especially in finding them from the natural
sources. In this study, by using Sulforhodamine B (SRB) colorimetric assay, compounds,
extracted from supermeal worm (Zophobas morio) larvae using two types of acidified organic
solvent (ethanol and isopropanol), were shown to inhibit the growth of a breast cancer line,
MCF-7. A comparative study of the effect was carried out on a normal cell line, Vero. Results
showed that, the two types of extracts inhibits growth of MCF-7 cell at varying degrees, on
the other hand, have much less effect on Vero cell. Extracts analysed by UV-vis spectroscopy,
showed peaks in the range of 260 to 280 nm, inferring the presence of aromatic amino acids,
whereas the highest peak of 3.608 AU at 230 nm indicates the presence of peptide bonds. By
Raman spectroscopy, peaks are observed at 1349 cm-1, 944 cm-1 and 841 cm-1 indicating the
presence of Tyr, Try and Gly, confirming the UV-vis analyses. All results of analyses implied
that the anticancer compounds contain peptides.
There is a paucity of information about the occurrence of microplastics (MPs) in edible fish tissues. Here, we investigated the potential presence of MPs in the excised organs (viscera and gills) and eviscerated flesh (whole fish excluding the viscera and gills) of four commonly consumed dried fish species (n = 30 per species). The MP chemical composition was then determined using micro-Raman spectroscopy and elemental analysis with energy-dispersive X-ray spectroscopy (EDX). Out of 61 isolated particles, 59.0% were plastic polymers, 21.3% were pigment particles, 6.55% were non-plastic items (i.e. cellulose or actinolite), while 13.1% remained unidentified. The level of heavy metals on MPs or pigment particles were below the detection limit. Surprisingly, in two species, the eviscerated flesh contained higher MP loads than the excised organs, which highlights that evisceration does not necessarily eliminate the risk of MP intake by consumers. Future studies are encouraged to quantify anthropogenic particle loads in edible fish tissues.
There are various approaches to enhancing the catalytic properties of TiO₂, including modifying its morphology by altering the surface reactivity and surface area of the catalyst. In this study, the primary aim is to enhance the photocatalytic activity by changing the TiO₂ nanotubes' architecture. The highly ordered infrastructure is favorable for a better charge carrier transfer. It is well known that anodization affects TiO₂ nanotubes' structure by increasing the anodization duration which in turn influence the photocatalytic activity. The characterizations were conducted by FE-SEM (fiend emission scanning electron microscopy), XRD (X-ray diffraction), RAMAN (Raman spectroscopy), EDX (Energy dispersive X-ray spectroscopy), UV-Vis (Ultraviolet visible spectroscopy) and LCMS/MS/MS (liquid chromatography mass spectroscopy). We found that the morphological structure is affected by the anodization duration according to FE-SEM. The photocatalytic degradation shows a photodegradation rate of k = 0.0104 min-1. It is also found that a mineralization of Simazine by our prepared TiO₂ nanotubes leads to the formation of cyanuric acid. We propose three Simazine photodegradation pathways with several intermediates identified.
A feasible production of poly (methyl methacrylate)@alloy (gold-silver) core shell has
been presented as candidate in enhanced detection of surface enhanced Raman scattering
(SERS). Free emulsifier- emulsion synthesised PMMA sphere with average size of 419 nm in
diameter were used as core material for incorporation of alloy nanoparticles (6 nm) resulting
a core-shell structure. The fabrication of PMMA@alloy SERS substrate was successfully
done via self-assembly thus the produced SERS substrate that comprise of unique optical
properties combination arising from periodic core arrangement and plasmonic activity of
alloy nanoparticles. Alloy is bimetallic nanoparticles in which the combination of silver
(Ag) and gold (Au) present an absolutely improved light resistance as compared to single
metal alone with great surface plasmon resonance. Morphology and elemental analysis was
performed through scanning electron microscope (SEM) and the analysis showing species of
both Au and Ag in single alloy nanoparticles. The alloy nanoparticles were also observed to
homogenously coating the PMMA sphere. Surface plasmon resonance activity was maximum
at 476 nm obtained from UV-Visible spectroscopy. High surface production was observed
to have periodically arranged PMMA@alloy core -shell and potentially to be used as SERS
substrate.
Surface functionalization of multi-walled carbon nanotubes (MWCNTs) was carried out using a gas phase treatment in a Universal Temperature Program (UTP) reactor by flowing SO3 gas onto the CNTs while being heated at different temperatures. The functionalized nanotubes were characterized using X-ray Fluorescence (XRF), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman spectroscopy. The amount of oxyen and sulfur containing groups was determined by acid-base titration. The titration results were in good agreement with elemental analysis using x-ray fluorescence. FTIRanalysis showed the presence of oxygen and sulfur containing groups, S=O, C-S, C=O and -COOH. Raman spectroscopy confirmed that oxygen and sulfur containing acidic groups covalently attached to the sidewall of the MWCNTs.