Electromagnetic (EM) waves transmitted by Horizontal Electric Dipole (HED) source to detect contrasts in subsurface resistivity termed Seabed Logging (SBL) is now an established method for hydrocarbon exploration. However, currently used EM wave detectors for SBL have several challenges including the sensitivity and its bulk size. This work exploits the benefit of superconductor technology in developing a magnetometer termed Superconducting Quantum Interference Device (SQUID) which can potentially be used for SBL. A SQUID magnetometer was fabricated using hexagon shape-niobium wire with YBa2Cu37O, (YBCO) as a barrier. The YBa2Cu37O, samples were synthesized by sol-gel method and were sintered using a furnace and conventional microwave oven. The YBCO gel was dried at 120 degrees C in air for 72 hours. It was then ground and divided into 12 parts. Four samples were sintered at 750 degrees C, 850 degrees C, 900 degrees C, and 950 degrees C for 12 hours in a furnace to find the optimum temperature. The other eight samples were sintered in a microwave with 1100 Watt (W) with a different sintering time, 5, 15, 45 minutes, 1 hour, 1 hour 15 minutes, 1 hour 30 minutes, 1 hour 45 minutes and 2 hours. A DEWAR container was designed and fabricated using fiberglass material. It was filled with liquid nitrogen (LN2) to ensure the superconducting state of the magnetometer. XRD results showed that the optimum sintering temperature for the formation of orthorhombic Y-123 phase was at 950 degrees C with the crystallite size of 67 nm. The morphology results from Field Emission Scanning Electron Microscopy (FESEM) showed that the grains had formed a rod shape with an average diameter of 60 nm. The fabricated SQUID magnetometer was able to show an increment of approximately 249% in the intensity of the EM waves when the source receiver offset was one meter apart.
The usefulness of carboxymethyl cellulose (CMC) as a matrix material in enhancing the controlled release formulations of bispyribac (BP) herbicide from the interlayer gallery of zinc hydroxide nitratesodium dodecylsulphate-bispyribac (ZHN-SDS-BP) nanocomposite was investigated. The CMC coated nanocomposite, ZHN-SDS-BP-CMC was characterised using several instruments for the determination of its physicochemical properties. The release rates of the BP were measured using a UV spectrophotometer, and the aqueous solutions containing PO3-₄ , SO2-₄ and Cl- were selected as release media in the release studies so as to mimic the real conditions of environmental soil. Significant release time delays, triggered by the gelation forming ability and hygroscopic nature of CMC, were observed in all release media, and the release processes were found to behave in a concentration-dependent manner in all release media. Fitting the release data into several kinetic models demonstrated that release in aqueous solutions of Na₃PO₄ and Na₂SO₄ was governed by pseudo second order processes, whereas the release in an aqueous NaCl solution was governed by the parabolic diffusion kinetic model. The potential of CMC in prolonging the release of BP from ZHN-SDS-BP-CMC can potentially help in reducing the pollution resulting from the overuse of pesticides.
Hybridization of beneficial organic guest with inorganic host affords scientists an opportunity to synthesize various combinations of new organic-inorganic nanohybrids with various potential applications, especially for controlled delivery of beneficial agent and storage. A new layered organic-inorganic nanohybrid material containing an agrochemical, 4-(2,4-dichlorophenoxy)butyrate (DPBA) in Zn-Al-layered double hydroxide inorganic interlayer was synthesised by direct and indirect methods. Both methods yielded mesoporous-type, phase pure, well-ordered layered nanohybrids with similar basal spacing of 28.5-28.7 angstroms and organic loading of around 54.3%. Compared to the material prepared by direct method, the ion exchanged product inherited more of the host's properties especially the pore structure and the organic moiety is also more easily released. This shows that the method of preparation plays an important role in determining the resulting physicochemical properties, in particular the release property and therefore can be used as a means to tune up the release property of the beneficial agent.
Layered organic-inorganic hybrid nanocomposite material was synthesised using 4-chlorophenoxyacetate (4CPA) as guest anion intercalated into the Zn-Al layered double hydroxide inorganic host by direct co-precipitation method at pH = 7.5 and Zn to Al molar ratio of 4. Both PXRD and FTIR results confirmed that the 4CPA was successfully intercalated into the Zn-AI-LDH interlayer. As a result, a well-ordered nanolayered organic-inorganic hybrid nanocomposite, with the expansion of the basal spacing from 8.9 angstroms in the layered double hydroxide to 20.1 angstroms in the resulting nanocomposite was observed. The FTIR spectrum of the nanocomposite (ZAC) showed that it composed spectral features of Zn-AI-LDH (ZAL) and 4CPA. The nanocomposites synthesized in this work are of mesoporous-type containing 39.8% (w/w) of 4CPA with mole fraction of Al3+ in the inorganic brucite-like layers (xAI) of 0.224. The release studies showed a rapid release of the 4CPA for the first 600 min, and more sustained thereafter. The total amount of 4CPA released from the nanocomposite interlayer into the aqueous solution were 21%, 66%, and 72% in 0.0001, 0.00025, and 0.0005 M sodium carbonate, respectively. In distilled water, about 75, 35, and 57% of 4CPA could be released in 1000 min, when the pH of the release media was set at 3, 6.25, and 12, respectively. In comparison with a structurally similar organic moiety with one more chlorine atom at the 2-position of the aromatic ring, namely 2,4-dichlorophenoxyacetate (24D), the 4CPA showed a slower release rate. The slightly bulkier organic moiety of 24D together with the presence of chlorine atom at the 2-position presumably had contributed to its higher release rate, and it seems that these factors may be exploited for tuning the release rate of intercalated guest anions with similar properties. This study suggests that layered double hydroxide can be used as a carrier for an active agent and the chemical structure of the intercalated moiety can be used to tune the desired release kinetics of the beneficial agent.
In this work, the direct electrochemistry of hemoglobin (Hb), which was immobilized on carbonyl functionalized single walled carbon nanotube (SWCNT) and deposited onto a gold (Au) electrode has been described. The synthesis of the network of crosslinked SWCNT/Hb was done with the help of crosslinking agent EDC (1-ethyl-3-(3-dimethylaminopropyl) carbodiimide). The UV-Vis and FTIR spectroscopy of SWCNT/Hb networks showed that Hb maintained its natural structure and kept good stability. In addition with this, scanning electron microscopy (SEM) illustrated that SWCNT/Hb networks had a featured layered structure and Hb being strongly liked with SWCNT surface. Cyclic voltammetry (CV) was used to study and to optimize the performance of the resulting modified electrode. The cyclic voltammetric (CV) responses of SWCNT/Hb networks in pH 7.0 exhibit prominent redox couple for the FeIII/II redox process with a midpoint potential of -0.46 V and -0.34, cathodic and anodic respectively. Furthermore, SWCNT/Hb networks are utilized for the detection of hydrogen peroxide (H2O2). Electrochemical measurements reveal that the resulting SWCNT/Hb electrodes display high electrocatalytic activity to H2O2 with high sensitivity, wide linear range, and low detection limit. Overall, the electrochemical results are due to excellent biocompatibility and excellent electron transport efficiency of CNT as well as high Hb loading and synergistic catalytic effect of the modified electrode toward H2O2.
A multiporous nanofiber (MPNFs) of SnO₂ and chitosan has been used for the immobilization of a redox protein, hemoglobin (Hb), onto the surface of glassy carbon electrode (GCE). The multiporous nanofiber of SnO₂ that has very high surface area is synthesized by using electrospinning technique through controlling the tin precursor concentration. Since the constructed MPNFs of SnO₂ exposes very high surface area, it increases the efficiency for biomolecule-loading. The morphology of fabricated electrodes is examined by SEM observation and the absorbance spectra of Hb/(MPNFs) of SnO₂ are studied by UV-Vis analysis. Cyclic Voltammetry and amperometry are employed to study and optimize the performance of the resulting fabricated electrode. After fabrication of the electrode with the Hb and MPNFs of SnO₂, a direct electron transfer between the protein's redox centre and the glassy carbon electrode was established. The modified electrode has showed a couple of redox peak located at -0.29 V and -0.18 V and found to be sensitive to H₂O₂. The fabricated electrode also exhibited an excellent electrocatalytic activity towards the reduction of H₂O₂. The catalysis currents increased linearly to the H₂O₂ concentration in a wide range of 5.0×10-6-1.5×10-4 M. Overall experimental results show that MPNFs of SnO₂ has a role towards the enhancement of the electroactivity of Hb at the electrode surface. Thus the MPNFs of SnO₂ is a very promising candidate for future biosensor applications.
In this study, a series of copper-ion-doped titanium dioxide (Cu-ion-doped TiO₂) nanotubes (NTs) were synthesized via a hydrothermal method by the concentration variation of doped Cu ions (0.00, 0.50, 1.00, 2.50, and 5.00 mmol). In addition, the samples were characterized using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), nitrogen gas adsorption measurements, and ultraviolet-visible (UV-Vis) diffuse-reflectance spectroscopy. The photocatalytic activity of the Cu-iondoped TiO₂ NTs was investigated for the degradation of methyl orange (MO) under sunlight. The results obtained from the structural and morphological studies revealed that, at low concentrations of Cu-doped TiO₂ NTs, Cu is incorporated into the interstitial positions of the TiO₂ lattice, affording a new phase of TiO₂ (hexagonal) instead of the anatase TiO₂ (tetragonal) observed for undoped TiO₂ NTs. EDX analysis confirmed the presence of Cu in the TiO₂-based photocatalyst. All of the investigated samples exhibited a hollow fibrous-like structure, indicative of an NT morphology. The inner and outer diameters of the NTs were 4 nm and 10 nm, respectively. The photocatalysts exhibited a large surface area due to the NT morphology and a type IV isotherm and H3 hysteresis, corresponding to the mesopores and slit-shaped pores. The Cu-ion-doped TiO₂ NTs were excited by sunlight because of their low bandgap energy; and after the incorporation of Cu ions into the interstitial positions of the TiO₂ lattice, the NTs exhibited high visible-light activity owing to the low bandgap.
The present study focuses on the microstructural and bioactive properties evolution in selective laser melting (SLM) β titanium alloys. We have applied cross-scan strategy for improving mechanical properties and lower elastic modulus of SLMed Ti-20Mg-5Ta alloys which has been shown to be altering the microstructure and refining the grain size. The cross-scan strategy can refine the microstructure and induce various deformation textures in contrast to the conventional scan strategy. The microstructures of Ti-20Mg-5Ta alloys indicate that the cross-scan strategy will yield the best mechanical properties and lower elastic modulus. The corrosion behavior of the Ti-20Mg-5Ta alloys was studied during immersion in an acellular simulated body fluid (SBF) at 37±0.50 °C for 28 days. Both the mechanical and bioactive properties showed that the novel Ti-20Mg-5Ta alloys should be ideal for bone implants.
Small sized electrocatalysts, which can be obtained by rapid nucleation and high supersaturation are imperative for outstanding methanol oxidation reaction (MOR). Conventional microwave synthesis processes of electrocatalysts include ultrasonication, stirring, pH adjustment, and microwave irradiation of the precursor mixture. Ethylene glycol (EG), which serves as a reductant and solvent was added during the ultrasonication or stirring stage. However, this step and pH adjustment resulted in unintended multi-stage gradual nucleation. In this study, the microwave reduction approach was used to induce rapid nucleation and high supersaturation in order to fabricate small-sized reduced graphene oxide-supported palladium (Pd/rGO) electrocatalysts via the delayed addition of EG, elimination of the pH adjustment step, addition of sodium carbonate (Na₂CO₃), prior microwave irradiation of the EG mixed with Na₂CO₃, and addition of room temperature precursor mixture. Besides its role as a second reducing agent, the addition of Na₂CO₃ was primarily intended to generate an alkaline condition, which is essential for the high-performance of electrocatalysts. Moreover, the microwave irradiation of the EG and Na₂CO₃ mixture generated highly reactive free radicals that facilitate rapid nucleation. Meanwhile, the room temperature precursor mixture increased supersaturation. Results showed improved electrochemically active surface area (78.97 m² g-1, 23.79% larger), MOR (434.49 mA mg-1, 37.96% higher) and stability.
Ga₂O₃/ITO/glass photoelectrodes prepared by the CVD method has rarely been tested in the electrochemical cell for water splitting. In this study, we investigate the photoelectrolytic performance of Ga₂O₃/ITO-glass photocatalysts produced by the high-temperature CVD route. The changing of N₂ carrier gas flow rate from 0 to 1800 seem induces change in the materials properties. XRD signal strength of the produced bi-phase Ga₂O₃ is observed to deteriorate, while diffraction line width broadens with increasing N₂ supply. Films show a combination of nanoclumps and nanostrips morphology. Ga/O ratio decreases, while the optical bandgap gradually increases from 4.37 to 4.42 eV with increasing O content and crystallite size. Photoluminescence measurements show UV, blue, green and red emissions, respectively. Linear sweep voltammetry of the electrodes in 0.1 M KOH electrolyte shows improvement in photocurrent density from 160 to 257 μA/cm² versus Ag/AgCl at 1 V bias, and a maximum photon-to-current conversion efficiency 0.06%.
Metanilate-layered double hydroxide nanohybrid compound was synthesized for controlled release purposes through co-precipitation method of the metal cations and organic anion. The effect of various divalent metal cations (M2+), namely Zn2+, Mg2+ and Ca2+ on the formation of metanilate-LDH nanohybrids, in which metanilate anion was intercalated into three different layered double hydroxide (LDH) systems; Zn-Al, Mg-Al and Ca-Al were investigated. The syntheses were carried out with M2+ to Al3+ initial molar ratio, R of 4. The pH of the mother liquor was maintained at pH 7.5 and 10 during the synthesis, and the resulting mixture was aged at around 70 degrees C for about 18 h. The intercalation of metanilate anion into the host was found to be strongly influenced by the M2+ that formed the inorganic metal hydroxide layers. Under our experimental condition, the formation of the nanohybrid materials was found to be more feasible for the Zn-Al than for the other two systems, in which the former showed well-ordered layered organic-inorganic nanohybrid structure with good crystallinity. Intercalation is confirmed by the expansion of the interlayer spacing to about 15-17 A when metanilate was introduced into the interlamellae of Zn-Al LDHs. In addition, CHNS and FTIR analyses also support that metanilate anion has been successfully intercalated into the interlamellae of the inorganic LDH. Apart from M2+, this study also shows that the initial pH of the mother liquor plays an important role in determining the physicochemical properties of the resulting nanohybrids, especially the mole fraction of the Zn2+ substituted by the Al3+ ion in the LDH inorganic sheets which in turn controlled the loading percentage of the organic anion, surface properties and the true density. Preliminary study shows that LDH can be used to host beneficial guests, active agent with controlled release capability of the guests. Generally the overall process is governed by pseudo second order kinetic but for the first 180 min, the release process can be slightly better described by parabolic diffusion than the other models.
Hydrotalcite-like inorganic layers of Zn-Al, a host containing an organic moiety, 2,4-dichlorophenoxy-acetate, as a guest, was prepared by the spontaneous self-assembly method from an aqueous solution for the formation of a new layered organic-inorganic hybrid nanocomposite material. In this synthesis, the host- and guest-forming species were simultaneously included in the mother liquor, aged, and separated. Various Zn/Al ratios (R = 2, 3, and 4), concentrations of 2,4-dichlorophenoxyacetic acid (0.03-0.1 M), and pH (7 and 10) were studied to optimize the formation of the layered nancomposite. It was found that the optimum conditions for the formation of the nanocomposite were R = 4, pH 7, and concentration of 2,4-dichlorophenoxyacetic acid = 0.08 M. X-ray diffraction shows that this sample affords a nanolayered structure with a basal spacing of 24.6 A.
Nanobiotechnology has emerged as a promising technology to develop new therapeutically active nanomaterials. The present study was aimed to biosynthesize AgNPs extracellularly using Aspergillus niger JX556221 fungal extract and to evaluate their anticancer potential against colon cancer cell line, HT-29. UV-visible spectral characterization of the synthesized AgNPs showed higher absorption peak at 440 nm wavelength. Transmission Electron Microscopy (TEM) analysis revealed the monodispersed nature of synthesized AgNPs occurring in spherical shape with a size in the range of 20-25 nm. Further, characterization using Energy Dispersive Spectroscopy (EDX) confirmed the face-centred cubic crystalline structure of metallic AgNPs. FTIR data revealed the occurrence of various phytochemicals in the cell free fungal extract which substantiated the fungal extract mediated AgNPs synthesis. The cytotoxic effect of AgNPs was studied by using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The results evidenced the cytotoxic effect of AgNPs on HT-29 cell lines in a dose dependent manner. The highest activity was found at 100 μg/ml concentration after 24 h of incubation. Use of propidium iodide staining examination method confirmed the cytotoxic effect of AgNPs through inducing cell apoptosis. AgNPs cytotoxicity was found to be through elevating reactive oxygen species (ROS), and caspase-3 activation resulting in induced apoptosis. Therefore, this research finding provides an insight towards the development of novel anticancer agents using biological sources.
In this study, performances of mesoporous Mo/Al2O3 catalysts prepared by sol-gel and post-hydrolysis methods in hydrocracking of atmospheric residual oil were compared. In addition, different methods: (i) the single step and (ii) conventional impregnation method to incorporate active metal over the mesoporous support were also investigated. For single step method, Mo/Al2O3 catalysts were synthesized directly by sol-gel and post-hydrolysis method. On the other hand, the impregnation method was a two step procedure which involved the production of alumina via sol-gel or post-hydrolysis method and followed by respective Mo impregnation. In general, mesoporous Mo/Al2O3 catalysts prepared by sol-gel method resulted in relatively higher surface area (> 400 m2/g) and large pore volume (- 0.8 cm3/g). Mo/Al2O3 catalysts prepared by sol-gel method exhibited higher hydrocracking activity as well. The Mo crystal size was found to relate directly with the hydrocracking result.
The substrate effects on surface morphologies, crystal structures, and magnetic properties of the sputter-deposited FePt thin films on Corning 1737, normal glass, and Si wafer substrates, respectively, were investigated. High in-plane coercivities of 10 kOe were obtained for the air-annealed films on Corning 1737 and Si wafer, where both films similarly have granular-like morphologies. Besides, increasing grain size and surface roughness of all the FePt films with the post-anneal temperature were observed. Moreover, partially separated grains were seen in the film on Si wafer, where the formation of Fe silicides during post-anneal is suspected, in which has enhanced the magnetic ordering.
This is our initial response towards preparation of nano-inductors garnet for high operating frequencies strontium iron garnet (Sr3Fe5O12) denoted as SrIG and yttrium iron garnet (Y3Fe5O12) denoted as YIG. The garnet nano crystals were prepared by novel sol-gel technique. The phase and crystal structure of the prepared samples were identified by using X-ray diffraction analysis. SEM images were done to reveal the surface morphology of the samples. Raman spectra was taken for yttrium iron garnet (Y3Fe5O12). The magnetic properties of the samples namely initial permeability (micro), relative loss factor (RLF) and quality factor (Q-Factor) were done by using LCR meter. From the XRD profile, both of the Y3Fe5O12 and Sr3Fe5O12 samples showed single phase garnet and crystallization had completely occurred at 900 degrees C for the SrIG and 950 degrees C for the YIG samples. The YIG sample showed extremely low RLF value (0.0082) and high density 4.623 g/cm3. Interesting however is the high Q factor (20-60) shown by the Sr3Fe5O12 sample from 20-100 MHz. This high performance magnetic property is attributed to the homogenous and cubical-like microstructure. The YIG particles were used as magnetic feeder for EM transmitter. It was observed that YIG magnetic feeder with the EM transmitter gave 39% higher magnetic field than without YIG magnetic feeder.
The fabrication of TiO2 nanotubes (TNT) was carried out by electrochemical anodization of Ti in aqueous electrolyte containing NH4F. The effect of electrolyte pH, applied voltage, fluoride concentration and anodization duration on the formation of TNT was investigated. It was observed that self-organized TNT can be formed by adjusting the electrolyte to pH 2-4 whereby applied voltage of 10-20 V can be performed to produce highly ordered, well-organized TNT. At 20 V, TNT can be fabricated in the concentration range of 0.07 M to 0.20 M NH4F. Higher fluoride concentration leads to etching of Ti surface and reveals the Ti grain boundaries. The prepared TNT films also show an increase in depth and in size with time and the growth of TNT films reach a steady state after 120 minutes. The morphology and geometrical aspect of the TNT would be an important factor influencing the photoelectrochemical response, with higher photocurrent response is generally associated with thicker layer of TNT. Consequently, one can tailor the resulting TNT to desired surface morphologies by simply manipulating the electrochemical parameters for wide applications such as solar energy conversion and photoelectrocatalysis.
The potential of using poly-(ethylene oxide)-block-distearoyl phosphatidyl-ethanolamine (mPEG-DSPE) polymer to prepare BDP-loaded micelles with high entrapment efficiency and mass median aerodynamic diameter of less than 5 microm demonstrating sustained release properties was evaluated. The result showed that lyophilized BDP-loaded polymeric micelles with entrapment efficiency of more than 96% could be achieved. Entrapment efficiency was affected by both the drug to polymer molar ratio and the amount of drug used. Investigation using FTIR and DSC confirmed that there was no chemical or physical interaction and the drug was molecularly dispersed within the micelles. TEM images showed that the drug-loaded polymeric micelles were spherical in shape with multivesicular morphology. Further analysis by photon correlation spectroscopy indicated that the particle size of the BDP-loaded micelles was about 22 nm in size. In vitro drug release showed a promising sustained release profile over six days following the Higuchi model. The mass median aerodynamic diameter and fine particle fraction were suitable for pulmonary delivery. Moreover, the small amount of deposited drug in the induction port (throat deposition) suggested possible reduction in incidence of oropharyngeal candidiasis, a side effect normally associated with inhaled corticosteroids therapy. The high encapsulation efficiency, comparable inhalation properties, sustained release behavior together with biocompatibility nature of the polymer support the potential of BDP-loaded polymeric micelles as a versatile delivery system to be used in the treatment of asthma and chronic obstructive pulmonary disease.
Well aligned TiO2 nanotubes were successfully synthesized by anodization of Ti foil at 60 V in a fluorinated bath comprised of ethylene glycol with 5 wt% of NH4F and 5 wt% of H2O2. In order to enhance the visible light absorption and photoelectrochemical response of pure TiO2 nanotube arrays, a mixed oxide system (W-TiO2) was investigated. W-TiO2 nanotube arrays were prepared using radio-frequency (RF) sputtering to incorporate the W into the lattice of TiO2 nanotube arrays. The W atoms occupy the substitutional position within the vacancies of TiO2 nanotube arrays. The as-anodized TiO2 is amorphous in nature while the annealed TiO2 is anatase phase. The mixed oxide (W-TiO2) system in suitable TiO2 phase plays important roles in efficient electron transfers due to the reduction in electron-hole recombination. In this article, the effect of the sputtered W into the as-anodized/annealed TiO2 nanotube arrays on the photoelectrochemical response was presented.
Shaped-controlled ZnO architectures including spherical, rod, rice-like and flower-like were fabricated via a reflux method in which the morphology, crystallinity, functional group and optical properties were tailored under different pH values in the precursor solution. The photoactivities of the prepared ZnO were evaluated under UV irradiation and the findings implied that the flower-like ZnO synthesized at pH 12 displayed superior activities on palm oil mil effluent degradation than those of other structures. The photocatalytic enhancement of flower-like ZnO was ascribed to its unique architecture, good crystallinity and superior optical properties. The flower-like ZnO with excellent photocatalytic performance have been confirmed by formation of hydroxyl radicals using a terephthalic acid-photoluminescence test. There was an optimal photocatalyst amount of 1.0 g/L, at which a maximum chemical oxygen demand removal of palm oil mill effluent was achieved under exposure of UV light. The phytotoxicity experiment via mung beans demonstrated a decrease in phytotoxicity.