The economics of bioflocculant production is coupled with the use of a low-cost substrate at appropriate culture conditions. The use of a waste substrate for this purpose offers an additional treatment measure to mitigate environmental pollution. We investigated the growth of Aspergillus flavus and its bioflocculant yield using chicken viscera hydrolysate as the sole media. The effects of culture conditions including time, pH, shaker speed, temperature and inoculum size on bioflocculant production were all investigated and optimised through response surface method based on the central component design (CCD) package of Design Expert. Next, the purified bioflocculant was physically and chemically characterised. Under optimised culture conditions (incubation time 72 h, pH 7, shaker speed 150 rpm, temperature 35 °C and inoculum 4%), 6.75 g/L yield of crude bioflocculant was recorded. The bioflocculant activity was mostly distributed in the cell-free supernatant with optimum efficiency of 91.8% at a dose of 4 mL/100 mL Kaolin suspension. The purified bioflocculant was a glycoprotein consisting of 23.46% protein and 74.5% sugar, including 46% neutral sugar and 2.01% uronic acid. The X-ray photoelectron spectroscopy fundamental analysis of the purified bioflocculant indicated that the mass proportion of C, O and N, were 63.46%, 27.87% and 8.86%, respectively. The bioflocculant is mainly composed of carbonyl, amino, hydroxyl, and amide functional groups. This study for the first time indicates a high potential of bioflocculant yield from chicken viscera at the appropriate culture conditions.
Sequentially precipitated Mg-promoted nickel-silica catalysts with ageing performed under various ultrasonic intensities were employed to study the catalyst performance in the partial hydrogenation of sunflower oil. Results from various characterisation studies showed that increasing ultrasonic intensity caused a higher degree of hydroxycarbonate erosion and suppressed the formation of Ni silicates and silica support, which improved Ni dispersion, BET surface area and catalyst reducibility. Growth of silica clusters on the catalyst aggregates were observed in the absence of ultrasonication, which explained the higher silica and nickel silicate content on the outer surface of the catalyst particle. Application of ultrasound also altered the electron density of the Ni species, which led to higher activity and enhanced product selectivity for sonicated catalysts. The catalyst synthesised with ultrasonic intensity of 20.78 Wcm-2 achieved 22.6% increase in hydrogenation activity, along with 28.5% decrease in trans-C18:1 yield at IV = 70, thus supporting the feasibility of such technique.
PtRu catalyst is a promising anodic catalyst for direct methanol fuel cells (DMFCs) but the slow reaction kinetics reduce the performance of DMFCs. Therefore, this study attempts to improve the performance of PtRu catalysts by adding nickel (Ni) and iron (Fe). Multiwalled carbon nanotubes (MWCNTs) are used to increase the active area of the catalyst and to improve the catalyst performance. Electrochemical analysis techniques, such as energy dispersive X-ray spectrometry (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS), are used to characterize the kinetic parameters of the hybrid catalyst. Cyclic voltammetry (CV) is used to investigate the effects of adding Fe and Ni to the catalyst on the reaction kinetics. Additionally, chronoamperometry (CA) tests were conducted to study the long-term performance of the catalyst for catalyzing the methanol oxidation reaction (MOR). The binding energies of the reactants and products are compared to determine the kinetics and potential surface energy for methanol oxidation. The FESEM analysis results indicate that well-dispersed nanoscale (2-5 nm) PtRu particles are formed on the MWCNTs. Finally, PtRuFeNi/MWCNT improves the reaction kinetics of anode catalysts for DMFCs and obtains a mass current of 31 A g(-1) catalyst.
H2S gas when exposed to metal can be responsible for both general and localized corrosion, which depend on several parameters such as H2S concentration and the corrosion product layer formed. Therefore, the formation of passive film on 316L steel when exposed to H2S environment was investigated using several analysis methods such as FESEM and STEM/EDS analyses, which identified a sulfur species underneath the porous structure of the passive film. X-ray photoelectron spectroscopy analysis demonstrated that the first layer of CrO3 and Cr2O3 was dissolved, accelerated by the presence of H2S-Cl-. An FeS2 layer was formed by incorporation of Fe and sulfide; then, passivation by Mo took place by forming a MoO2 layer. NiO, Ni(OH)2, and NiS barriers are formed as final protection for 316L steel. Therefore, Ni and Mo play an important role as a dual barrier to maintain the stability of 316L steel in high pH2S environments. For safety concern, this paper is aimed to point out a few challenges dealing with high partial pressure of H2S and limitation of 316L steel under highly sour condition for the oil and gas production system.
We use two-dimensional electronic spectroscopy to measure the ultrafast correlation dynamics between the Q x and Q y transitions in chlorophyll molecules. We derive a variation to the center line slope method to quantify the frequency fluctuation cross-correlation function, C xy( Tw). Compared with the frequency fluctuation correlation function of the Q y transition, we observe that there is only a minimal correlation between the Q x and Q y transition, even at the ultrashort timescale of ∼100 fs, which then decays to zero in a time scale of ∼2 ps.
In the present study, the construction of arrays on silicon for naked-eye detection of DNA dengue was demonstrated. The array was created by exposing a polyethylene glycol (PEG) silane monolayer to 254 nm ultraviolet (UV) light through a photomask. Formation of the PEG silane monolayer and photomodifed surface properties was thoroughly characterized by using atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements. The results of XPS confirmed that irradiation of ultraviolet (UV) light generates an aldehyde functional group that offers conjugation sites of amino DNA probe for detection of a specific dengue virus target DNA. Employing a gold enhancement process after inducing the electrostatic interaction between positively charged gold nanoparticles and the negatively charged target DNA hybridized to the DNA capture probe allowed to visualize the array with naked eye. The developed arrays demonstrated excellent performance in diagnosis of dengue with a detection limit as low as 10 pM. The selectivity of DNA arrays was also examined using a single base mismatch and noncomplementary target DNA.
Hybrid gold nanostructures seeded into nanotextured zinc oxide (ZnO) nanoflowers (NFs) were created for novel biosensing applications. The selected 'spotted NFs' had a 30-nm-thick gold nanoparticle (AuNP) layer, chosen from a range of AuNP thicknesses, sputtered onto the surface. The generated nanohybrids, characterized by morphological, physical and structural analyses, were uniformly AuNP-seeded onto the ZnO NFs with an average length of 2-3 μm. Selective capture of molecular probes onto the seeded AuNPs was evidence for the specific interaction with DNA from pathogenic Leptospirosis-causing strains via hybridization and mis-match analyses. The attained detection limit was 100 fM as determined via impedance spectroscopy. High levels of stability, reproducibility and regeneration of the sensor were obtained. Selective DNA immobilization and hybridization were confirmed by nitrogen and phosphorus peaks in an X-ray photoelectron spectroscopy analysis. The created nanostructure hybrids illuminate the mechanism of generating multiple-target, high-performance detection on a single NF platform, which opens a new avenue for array-based medical diagnostics.
The aim of this study was to determine the surface chemistry during biocorrosion process on growth and on the production of exopolymeric substances (EPS) in batch cultures of mix-strains of marine sulphate-reducing bacteria (SRB) isolated from Malaysian Shipyard and Engineering Harbours, Pasir Gudang. The EPS and precipitates were analyzed by x-ray photoelectron spectroscopy (XPS). The XPS results indicate that Fe(2p3/2) spectrum for iron sulphide can be fitted with Fe(II) and Fe(III) components, both corresponding to Fe-S bond types. The absence of oxide oxygen in the O(1s) spectrum and Fe(III)-O bond types in the Fe(2p3/2) spectrum supports the conclusion that iron sulphides are composed of both ferric and ferrous iron coordinated with monosulphide and disulphide.
Chemical structure of treated and untreated Aciplex membrane has been studied by X-ray Photoelectron Spectroscopy (XPS). Survey spectra showed that both membrane surfaces consist of Fluorine, Carbon, Oxygen, Sulphur and trace of Titanium. Binding energies for the elements are (C1s at 290.6 eV, F1s at 687.5 eV, O1s at 531.3 eV, S2P at 168.1 eV and Ti2P at 454.4 eV). Analysis of narrow scan XPS-spectra of each element demonstrate the presence of (-CF, -CF2, CF3, C-O-C and SO-3) groups, which are in agreement with the structural formula as disclosed by the manufacturer. There is no significant change in chemical states of untreated and treated membrane, which reflect its stability to treatment conditions.
Struktur kimia Aciplex membran yang sudah dibersihkan dan yang belum dibersihkan telah dikaji menggunakan Spektroskopi Fotoelektron Sinaran-X (XPS). Spektra yang telah ditinjau menunjukkan bahawa kedua-dua permukaan membran mengandungi Florin, Karbon, Oksigen, Sulfur dan sedikit Titanium. Tenaga ikatan bagi unsur-unsur tersebut adalah (C1s pada 290.6 eV, F1s pada 687.5 eV. O1s pada 531.3 eV, S2P pada 168.2 eV dan Ti2P pada 454.4 eV). Analisis imbasan kecil spektra-xps bagi setiap unsur menunjukkan kehadiran kilmpulan (-CF, - CF2, CF3, C-O-C dan SO-3) yang bertepatan dengan formula struktur dari pihak pembekal. Tiada terdapat perubahan nyata berhubung dengan keadaan kimia membran yang sudah dibersihkan dan yang belum dibersihkan yang menggambarkan kestabilannya terhadap keadaan pembersihan.
Microbial content formed in bioreactors plays a significant role in the anaerobic process. Therefore, the physicochemical characteristics of microbial content in a modified anaerobic inclining-baffled reactor (MAI-BR) treating recycled paper mill effluent (RPME) were investigated using Fourier transform infrared (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetric (TG), and derivative thermogravimetric (DTG) analyses, scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), Brunauer-Emmett-Teller (BET), and surface area analyzer. FTIR spectra revealed that the microbial content had stronger characteristic peaks corresponding to alcohols, water, lipids carbohydrates, proteins, and mineral compounds. Calcite, muscovite, and lepidolite were the prevalent mineral phases found by XRD analysis. The elemental of these minerals like C, Ca, N, O, and Si was confirmed by XPS results. The microbial content samples from each compartment showed similar thermal behavior. SEM images showed that straight rod-shaped and Methanosaeta-like microorganisms were predominant, whereas C, O, and Ca were noticed by EDS on the surface of granules. The BET surface areas and pores of granules are found to decline throughout the reactor's compartment, where Compartment 1 had the largest values. Thus, the findings of this study establish further understanding of the physicochemical properties of microbial content formed in MAI-BR during the RPME treatment.
A chemical method to synthesize amorphous silica nanoparticles from the incinerated paddy straw has been introduced. The synthesis was conducted through the hydrolysis by alkaline-acidic treatments. As a result, silica particles produced with the sizes were ranging at 60-90 nm, determined by high-resolution microscopy. The crystallinity was confirmed by surface area electron diffraction. Apart from that, chemical and diffraction analyses for both rice straw ash and synthesized silica nanoparticles were conducted by X-ray diffraction and Fourier-transform infrared spectroscopy. The percentage of silica from the incinerated straw was calculated to be 28.3. The prominent surface chemical bonding on the generated silica nanoparticles was with Si-O-Si, stretch of Si-O and symmetric Si-O bonds at peaks of 1090, 471, and 780 cm-1, respectively. To confirm the impurities of the elements in the produced silica, were analyzed using X-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy. The stability of silica nanoparticles was investigated using thermogravimetric analysis and zeta potential. The measured size from zeta potential analysis was 411.3-493 nm and the stability of mass reduction was located at 200 °C with final amount of mass reduced ∼88% and an average polydispersity Index was 0.195-0.224.
In this study, silver (Ag) and cobalt oxide (Co3O4) decorated polyaniline (PANI) fibers were prepared by the combination of in-situ aniline oxidative polymerization and the hydrothermal methodology. The morphology of the prepared Ag/Co3O4@PANI ternary nanocomposite was studied by scanning electron microscopy and transmission electron microscopy, while the structural studies were carried out by X-ray diffraction and X-ray photoelectron spectroscopy. The morphological characterization revealed fibrous shaped PANI, coated with Ag and Co3O4 nanograins, while the structural studies revealed high purity, good crystallinity, and slight interactions among the constituents of the Ag/Co3O4@PANI ternary nanocomposite. The electrochemical performance studies revealed the enhanced performance of the Ag/Co3O4@PANI nanocomposite due to the synergistic/additional effect of Ag, Co3O4 and PANI compared to pure PANI and Co3O4@PANI. The addition of the Ag and Co3O4 provided an extended site for faradaic reactions leading to the high specific capacity. The Ag/Co3O4@PANI ternary nanocomposite exhibited an excellent specific capacity of 262.62 C g-1 at a scan rate of 3 mV s-1. The maximum energy and power density were found to be 14.01 Wh kg-1 and 165.00 W kg-1, respectively. The cyclic stability of supercapattery (Ag/Co3O4@PANI//activated carbon) consisting of a battery type electrode demonstrated a gradual increase in specific capacity with a continuous charge-discharge cycle until ~1000 cycles, then remained stable until 2500 cycles and later started decreasing, thereby showing the cyclic stability of 121.03% of its initial value after 3500 cycles.
In this study, ternary composites of polyaniline (PANI) with manganese dioxide (MnO2) nanorods and carbon nanotubes (CNTs) were prepared by employing a hydrothermal methodology and in-situ oxidative polymerization of aniline. The morphological analysis by scanning electron microscopy showed that the MnO2 possessed nanorod like structures in its pristine form, while in the ternary PANI@CNT/MnO2 composite, coating of PANI over CNT/MnO2, rods/tubes were evidently seen. The structural analysis by X-ray diffraction and X-ray photoelectron spectroscopy showed peaks corresponding to MnO2, PANI and CNT, which suggested efficacy of the synthesis methodology. The electrochemical performance in contrast to individual components revealed the enhanced performance of PANI@CNT/MnO2 composite due to the synergistic/additional effect of PANI, CNT and MnO2 compared to pure MnO2, PANI and PANI@CNT. The PANI@CNT/MnO2 ternary composite exhibited an excellent specific capacity of 143.26 C g-1 at a scan rate of 3 mV s-1. The cyclic stability of the supercapattery (PANI@CNT/MnO2/activated carbon)-consisting of a battery type electrode-demonstrated a gradual increase in specific capacity with continuous charge-discharge over ~1000 cycles and showed a cyclic stability of 119% compared to its initial value after 3500 cycles.
In this study, nano- and microsized zinc oxide (ZnO) materials were doped with different manganese (Mn) contents (1-5 mol%) via a simple sol-gel method. The structural, morphological, optical and chemical environments of the materials were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), UV-visible spectroscopy (UV-vis) and X-ray photoelectron spectroscopy (XPS). XRD results revealed that all synthesised materials were pure and single phased with a hexagonal wurtzite structure of ZnO. However, at a low annealing temperature, a nanorod-like shape can be obtained for all Zn(1-x)MnxO materials. In addition, EDX spectra confirmed the presence of Mn in the ZnO lattice and the atomic percentage was nearly equal to the calculated stoichiometry. UV-vis spectroscopy further revealed that materials in nano size exhibited band gap widening with an increase of the Mn content in the ZnO lattice. In contrast, micron state materials exhibited band gap narrowing with increasing Mn content up to 3% and then begin to widen when Mn > 3%. This is because the band gaps of these materials are affected by the dimensions of the crystals and the Mn content in the materials. Furthermore, XPS results revealed the existence of multiple states of Mn in all synthesised materials. By combining the information obtained from UV-vis and the XPS valence band, shifting in the valence band maximum (VBM) and conduction band minimum (CBM) was observed. Based on XPS results, the calculation of density functional theory studies revealed that the presence of Mn2+, Mn3+, and Mn4+ ions in the materials influences the band gap changes. It was also revealed that the nanosized Zn0.99Mn0.01O exhibited a higher photocatalytic activity than the other samples for degrading methylene blue (MB) dyes, owing to its smallest crystallite size.
The effects of different post-deposition annealing ambients (oxygen, argon, forming gas (95% N2 + 5% H2), and nitrogen) on radio frequency magnetron-sputtered yttrium oxide (Y2O3) films on n-type gallium nitride (GaN) substrate were studied in this work. X-ray photoelectron spectroscopy was utilized to extract the bandgap of Y2O3 and interfacial layer as well as establishing the energy band alignment of Y2O3/interfacial layer/GaN structure. Three different structures of energy band alignment were obtained, and the change of band alignment influenced leakage current density-electrical breakdown field characteristics of the samples subjected to different post-deposition annealing ambients. Of these investigated samples, ability of the sample annealed in O2 ambient to withstand the highest electric breakdown field (approximately 6.6 MV/cm) at 10-6 A/cm2 was related to the largest conduction band offset of interfacial layer/GaN (3.77 eV) and barrier height (3.72 eV).
Band gap change in doped ZnO is an observed phenomenon that is very interesting from the fundamental point of view. This work is focused on the preparation of pure and single phase nanostructured ZnO and Cu as well as Mn-doped ZnO for the purpose of understanding the mechanisms of band gap narrowing in the materials. ZnO, Zn0.99Cu0.01O and Zn0.99Mn0.01O materials were prepared using a wet chemistry method, and X-ray diffraction (XRD) results showed that all samples were pure and single phase. UV-visible spectroscopy showed that materials in the nanostructured state exhibit band gap widening with respect to their micron state while for the doped compounds exhibited band gap narrowing both in the nano and micron states with respect to the pure ZnO materials. The degree of band gap change was dependent on the doped elements and crystallite size. X-ray photoelectron spectroscopy (XPS) revealed that there were shifts in the valence bands. From both UV-visible and XPS spectroscopy, it was found that the mechanism for band gap narrowing was due to the shifting of the valance band maximum and conduction band minimum of the materials. The mechanisms were different for different samples depending on the type of dopant and dimensional length scales of the crystallites.
The photochemical synthesis of two-dimensional (2D) nanostructured from semiconductor materials is unique and challenging. We report, for the first time, the photochemical synthesis of 2D tin di/sulfide (PS-SnS₂-x, x = 0 or 1) from thioacetamide (TAA) and tin (IV) chloride in an aqueous system. The synthesized PS-SnS₂-x were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), a particle size distribution analyzer, X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FTIR), thermal analysis, UV⁻Vis diffuse reflectance spectroscopy (DR UV⁻Vis), and photoluminescence (PL) spectroscopy. In this study, the PS-SnS₂-x showed hexagonally closed-packed crystals having nanosheets morphology with the average size of 870 nm. Furthermore, the nanosheets PS-SnS₂-x demonstrated reusable photo-degradation of methylene blue (MB) dye as a water pollutant, owing to the stable electronic conducting properties with estimated bandgap (Eg) at ~2.5 eV. Importantly, the study provides a green protocol by using photochemical synthesis to produce 2D nanosheets of semiconductor materials showing photo-degradation activity under sunlight response.
SnO₂ nanoparticle production using thermal treatment with tin(II) chloride dihydrate and polyvinylpyrrolidone capping agent precursor materials for calcination was investigated. Samples were analyzed using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), energy dispersive X-ray (EDX), transmission electron microscopy (TEM), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), diffuse UV-vis reflectance spectra, photoluminescence (PL) spectra and the electron spin resonance (ESR). XRD analysis found tetragonal crystalline structures in the SnO₂ nanoparticles generated through calcination. EDX and FT-IR spectroscopy phase analysis verified the derivation of the Sn and O in the SnO₂ nanoparticle samples from the precursor materials. An average nanoparticle size of 4–15.5 nm was achieved by increasing calcination temperature from 500 °C to 800 °C, as confirmed through TEM. The valence state and surface composition of the resulting nanoparticle were analyzed using XPS. Diffuse UV-vis reflectance spectra were used to evaluate the optical energy gap using the Kubelka-Munk equation. Greater calcination temperature resulted in the energy band gap falling from 3.90 eV to 3.64 eV. PL spectra indicated a positive relationship between particle size and photoluminescence. Magnetic features were investigated through ESR, which revealed the presence of unpaired electrons. The magnetic field resonance decreases along with an increase of the g-factor value as the calcination temperature increased from 500 °C to 800 °C. Finally, Escherichia coli ATCC 25922 Gram (–ve) and Bacillus subtilis UPMC 1175 Gram (+ve) were used for in vitro evaluation of the tin oxide nanoparticle’s antibacterial activity. This work indicated that the zone of inhibition of 22 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.
The performance of a modified electrode of nanocomposite films consisting of polypyrrole-chitosan-titanium dioxide (Ppy-CS-TiO₂) has been explored for the developing a non-enzymatic glucose biosensors. The synergy effect of TiO₂ nanoparticles (NPs) and conducting polymer on the current responses of the electrode resulted in greater sensitivity. The incorporation of TiO₂ NPs in the nanocomposite films was confirmed by X-ray photoelectron spectroscopy (XPS) spectra. FE-SEM and HR-TEM provided more evidence for the presence of TiO₂ in the Ppy-CS structure. Glucose biosensing properties were determined by amperommetry and cyclic voltammetry (CV). The interfacial properties of nanocomposite electrodes were studied by electrochemical impedance spectroscopy (EIS). The developed biosensors showed good sensitivity over a linear range of 1-14 mM with a detection limit of 614 μM for glucose. The modified electrode with Ppy-CS nanocomposite also exhibited good selectivity and long-term stability with no interference effect. The Ppy-CS-TiO₂ nanocomposites films presented high electron transfer kinetics. This work shows the role of nanomaterials in electrochemical biosensors and describes the process of their homogeneous distribution in composite films by a one-step electrochemical process, where all components are taken in a single solution in the electrochemical cell.
In this work, advanced nanoscale surface characterization of CuO Nanoflowers synthesized by controlled hydrothermal approach for significant enhancement of catalytic properties has been investigated. The CuO nanoflower samples were characterized by field-emission scanning electron microscopy (FE-SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, high-resolution transmission electron microscopy (HR-TEM), selected-area electron diffraction (SAED), high-angular annular dark field scanning transmission electron microscopy (HAADF-STEM) with elemental mapping, energy dispersive spectroscopy (STEM-EDS) and UV-Vis spectroscopy techniques. The nanoscale analysis of the surface study of monodispersed individual CuO nanoflower confirmed the fine crystalline shaped morphology composed of ultrathin leaves, monoclinic structure and purified phase. The result of HR-TEM shows that the length of one ultrathin leaf of copper oxide nanoflower is about ~650-700 nm, base is about ~300.77 ± 30 nm and the average thickness of the tip of individual ultrathin leaf of copper oxide nanoflower is about ~10 ± 2 nm. Enhanced absorption of visible light ~850 nm and larger value of band gap energy (1.68 eV) have further supported that the as-grown material (CuO nanoflowers) is an active and well-designed surface morphology at the nanoscale level. Furthermore, significant enhancement of catalytic properties of copper oxide nanoflowers in the presence of H2O2 for the degradation of methylene blue (MB) with efficiency ~96.7% after 170 min was obtained. The results showed that the superb catalytic performance of well-fabricated CuO nanoflowers can open a new way for substantial applications of dye removal from wastewater and environment fields.